CN107879943B - Iron-based complex and application thereof - Google Patents
Iron-based complex and application thereof Download PDFInfo
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- CN107879943B CN107879943B CN201710952823.8A CN201710952823A CN107879943B CN 107879943 B CN107879943 B CN 107879943B CN 201710952823 A CN201710952823 A CN 201710952823A CN 107879943 B CN107879943 B CN 107879943B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/14—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton from compounds containing already amino and carboxyl groups or derivatives thereof
- C07C227/18—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton from compounds containing already amino and carboxyl groups or derivatives thereof by reactions involving amino or carboxyl groups, e.g. hydrolysis of esters or amides, by formation of halides, salts or esters
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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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/223—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material containing metals, e.g. organo-metallic compounds, coordination complexes
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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
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C229/00—Compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C229/76—Metal complexes of amino carboxylic acids
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N21/643—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" non-biological material
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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
- C02F2101/103—Arsenic compounds
Abstract
The invention discloses an iron-based complex and application thereof, and a preparation method of the iron-based complex comprises the following steps: with 2-aminoterephthalic acid and FeCl3·6H2O as raw material, N-dimethyl formamide as solvent, 1.3838mmol FeCl per 1.3838mmol 2-amino terephthalic acid3·6H2Ratio of O to 30mL of Nitrogen-Nitrogen dimethylformamide 2-amino terephthalic acid and FeCl3·6H2Dissolving O in N-N dimethyl formamide, and then preparing the iron-based complex by adopting a hydrothermal reaction. The iron-based complex can be used for detecting the concentration of arsenate ions in a water body and can also be used for removing the arsenate ions in the water body. The method can not only quickly detect the concentration of the arsenate ions in the water body and has high detection sensitivity, but also can effectively remove the arsenate ions in the water body.
Description
Technical Field
The invention relates to the technical field of detection and removal of arsenate ions in water, in particular to an iron-based complex and application thereof.
Background
Arsenate ions are one of the most toxic and carcinogenic substances and are widely present in the environment such as atmosphere, water, soil, organisms and the like. Geological factors such as volcanic eruption, efflorescence reaction, biological activity, corrosion of rock soil and the like all cause arsenic pollution in water and soil, and human activities such as smelting of arsenic-containing minerals, use of arsenic-containing pesticides and preservatives, and combustion of fossil fuels cause arsenic pollution to the environment. If people are exposed to arsenic-polluted water for a long time, the arsenic-polluted water can have serious influence on human health, and easily induce diseases such as skin lesion, congenital malformation, nephropathy, liver function injury, leukemia, atherosclerosis, cancer and the like, and even death. Due to the crisis caused by arsenic pollution and public water quality concerns, the world health organization stipulates that the concentration limit of arsenic in human-drinking water sources is 10 mug/L, so that the detection and removal of arsenate ions in water and other environments are always research hotspots in the field.
In the prior art, continuous fluorescence method, colorimetric method and electrochemical technology are usually adopted to detect arsenate ions in water, and adsorption method, flocculation method and chemical oxidation method are adopted to remove the arsenate ions in the water, but the methods only have single detection or removal function, and the method for detecting the arsenate ions has low speed and low detection sensitivity, and the method for removing arsenic has undesirable removal effect on the arsenate ions.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the iron-based complex and the application thereof, which not only can rapidly detect the concentration of the arsenate ions in the water body and have high detection sensitivity, but also can effectively remove the arsenate ions in the water body.
The purpose of the invention is realized by the following technical scheme:
an iron-based complex, the preparation method of which comprises the following steps: with 2-aminoterephthalic acid and FeCl3·6H2O as raw material, N-dimethyl formamide as solvent, 1.3838mmol FeCl per 1.3838mmol 2-amino terephthalic acid3·6H2Ratio of O to 30mL of Nitrogen-Nitrogen dimethylformamide 2-amino terephthalic acid and FeCl3·6H2Dissolving O in N-N dimethyl formamide, and then preparing the iron-based complex by adopting a hydrothermal reaction.
Preferably, the iron-based complex prepared by hydrothermal reaction comprises: when 2-amino terephthalic acid and FeCl3·6H2Dissolving O in N-N dimethylformamide, placing the mixture in an environment of 120 ℃ for hydrothermal reaction for 20-24 hours, then carrying out solid-liquid separation, cleaning the solid obtained by the solid-liquid separation, and carrying out freeze drying for 48 hours to obtain the iron-based complex.
Preferably, the washing the solid obtained by the solid-liquid separation comprises the following steps: and respectively cleaning the solid obtained by solid-liquid separation for multiple times by adopting nitrogen-nitrogen dimethylformamide and ethanol.
The application of the iron-based complex is used for detecting the concentration of arsenate ions in a water body.
Preferably, the detection range of the iron-based complex to the concentration of arsenate ions in the water body is 0.1-50 mu mol/L per 5mg of the iron-based complex.
The application of the iron-based complex is used for removing arsenate ions in a water body.
Preferably, when the arsenate ions in the water body are removed, the dosage of the iron-based complex is 0.2g/L, the pH value of the water body is controlled to be 6, and the treatment time is controlled to be 24 hours.
The application of the iron-based complex is used for detecting the concentration of the arsenate ions in the water body and removing the arsenate ions in the water body.
According to the technical scheme provided by the invention, 1.3838mmol FeCl is used for every 1.3838mmol of 2-aminoterephthalic acid in the iron-based complex provided by the invention3·6H2Ratio of O to 30mL of Nitrogen-Nitrogen dimethylformamide 2-amino terephthalic acid and FeCl3·6H2O is dissolved in N-N dimethyl formamide and then prepared by hydrothermal reaction, so that the iron-based complex can be used for detecting the concentration of arsenate ions in waterAnd the double functions of removing the arsenate ions in the water body, the problem of single function of detecting the arsenate ions and removing the arsenate ions in the prior art is solved, the arsenate ions in the water body can be pre-enriched, the detection speed is high, the detection sensitivity is high, the detection range is wide, the detection limit is low, an alarm is given before the concentration of the arsenate ions in the water body reaches the maximum limit value, the arsenate ions in the water body can be effectively removed, and the harm of the arsenate ion pollution to the environment and human beings is effectively reduced.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on the drawings without creative efforts.
FIG. 1 is a schematic drawing of a scanning electron microscope and a schematic drawing of a transmission electron microscope of an iron-based complex provided in example 1 of the present invention.
FIG. 2 provides an X-ray diffraction pattern of an iron-based complex according to example 1 of the present invention.
FIG. 3 is a schematic diagram of fluorescence intensity obtained by performing concentration fluorescence detection on a water body with an arsenate ion concentration of 0.1-50 μmol/L by using the iron-based complex provided in embodiment 1 of the present invention.
Fig. 4 is a schematic diagram of fluorescence performance obtained by fluorescence detection of the iron-based complex on the concentration of arsenate ions in a water body in which other cations or anions exist according to embodiment 1 of the present invention.
Fig. 5 is a schematic diagram of the effect of the iron-based complex on removing arsenate ions in water bodies with different arsenate ion concentrations in embodiment 1 of the present invention.
FIG. 6 is a schematic diagram of the effect of the iron-based complex on removing arsenate ions from a water body at different time points according to embodiment 1 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without making any creative effort, shall fall within the protection scope of the present invention.
The iron-based complex provided by the present invention and its use are described in detail below. Details which are not described in detail in the embodiments of the invention belong to the prior art which is known to the person skilled in the art.
An iron-based complex, the preparation method of which comprises the following steps: with 2-aminoterephthalic acid and FeCl3·6H2O as raw material, N-dimethyl formamide as solvent, 1.3838mmol FeCl per 1.3838mmol 2-amino terephthalic acid3·6H2Ratio of O to 30mL of Nitrogen-Nitrogen dimethylformamide 2-amino terephthalic acid and FeCl3·6H2Dissolving O in N-N dimethyl formamide, and then preparing the iron-based complex by adopting a hydrothermal reaction.
Specifically, the preparation method of the iron-based complex provided by the invention can comprise the following embodiments:
(1) 2-amino terephthalic acid, FeCl3·6H2The use ratio of the O to the nitrogen-nitrogen dimethylformamide is preferably 1.3838mmol, 1.3838mmol and 30mL, and the use ratio not only can enable the prepared iron-based complex to have higher detection sensitivity on the concentration of the arsenate ions in the water body, but also can effectively improve the removal effect on the arsenate ions in the water body.
(2) 2-amino terephthalic acid and FeCl3·6H2Placing O in N-dimethylformamide, preferably performing ultrasonic treatment for 5min, and stirring for 2 hr to obtain 2-amino terephthalic acid and FeCl3·6H2O decomposes substantially uniformly in nitrogen-nitrogen dimethylformamide.
(3) The iron-based complex prepared by adopting the hydrothermal reaction comprises the following components: when 2-amino terephthalic acid and FeCl3·6H2Dissolving O in N-dimethylformamide, and placing in an environment of 120 ℃ for 20-24 hoursAnd (3) carrying out hydrothermal reaction, cooling to room temperature, carrying out solid-liquid separation, cleaning the solid obtained by the solid-liquid separation, and carrying out freeze drying for 48 hours to obtain the octahedral iron-based complex. By controlling the reaction temperature of the hydrothermal reaction at 120 ℃ and controlling the reaction time of the hydrothermal reaction at 20-24 hours, the detection sensitivity of the prepared iron-based complex on the concentration of the arsenate ions in the water body is higher, and the removal effect of the arsenate ions in the water body can be effectively improved. The solid obtained by solid-liquid separation is cleaned and then is frozen and dried, so that the appearance of the prepared iron-based complex can be adjusted, the performance of the prepared iron-based complex is more stable, and the repetition rate is higher. In practical application, when 2-amino terephthalic acid and FeCl3·6H2Dissolving O in nitrogen-nitrogen dimethyl formamide, placing the nitrogen-nitrogen dimethyl formamide into a reaction kettle, placing the reaction kettle into a blast drying box, carrying out hydrothermal reaction for 20-24 hours at 120 ℃, taking out suspension in the reaction kettle after cooling to room temperature, carrying out centrifugal separation, respectively washing solids obtained by solid-liquid separation by using nitrogen-nitrogen dimethyl formamide and ethanol for multiple times, and finally placing the solids in a freeze drying device for freeze drying for 48 hours, thereby obtaining the iron-based complex with the octahedral structure.
Further, the iron-based complex provided by the invention has double functions of detecting the concentration of arsenate ions in the water body and removing the arsenate ions in the water body:
(1) the method is used for detecting the concentration of arsenate ions in the water body: when the concentration of the arsenate ions in the water body is detected by adopting a fluorescence spectrometry, the pH value of the water body is controlled to be 6-8, the concentration of the arsenate ions in the water body can be quickly detected by adopting the iron-based complex provided by the invention as a detection agent, and the detection range of the concentration of the arsenate ions in the water body is 0.1-50 mu mol/L for every 5Mg of the iron-based complex, even if the iron-based complex contains Mg2+、Al3+、Bi3+、Ag+、Cu2+、Co2+、Zn2+、Ni2+、Mn2+、Pb2+、Cr3+Isocation and containing Ac-、SO4 2-、HCO3 -、CO3 2-、NO3 -、Cl-、Br-In the water body with anions, the detection of the iron-based complex on the concentration of the arsenate ions in the water body can still reach the detection speed and the detection precision when no interfering ions exist, so that the iron-based complex provided by the invention can pre-enrich the arsenate ions in the water body, has higher detection sensitivity, wider detection range and lower detection limit on the concentration of the arsenate ions in the water body, and can realize good rapid selective detection.
(2) Used for removing arsenate ions in water: when the arsenate ions in the water body are removed, the iron-based complex provided by the invention is used as an adsorbent, the dosage of the iron-based complex is preferably 0.2g/L, the pH value of the water body is preferably controlled to be 6, and the removal treatment time is preferably controlled to be 24 hours, so that the maximum adsorption removal of the arsenate ions in the water body can be realized, and the aim of effectively removing the arsenate ions in the water body is fulfilled; according to the Langmuir adsorption model, the maximum removal amount of the arsenate ions in the water body by the iron-based complex provided by the invention can be calculated to be 125mg/g, so that the harm of arsenic pollution to the environment and human is effectively reduced.
In conclusion, the embodiment of the invention has the advantages of simple preparation method, easy operation, high mass transfer rate and the like, has double functions of detecting the concentration of the arsenate ions in the water body and removing the arsenate ions in the water body, overcomes the problem of single function of detecting the arsenate ions and removing the arsenate ions in the water body in the prior art, can pre-enrich the arsenate ions in the water body, quickly detects the concentration of the arsenate ions in the water body, has high detection sensitivity, wide detection range and low detection limit, gives an alarm before the concentration of the arsenate ions in the water body reaches the maximum limit value, and can effectively remove the arsenate ions in the water body, thereby reducing the harm to the environment and human caused by the pollution of the arsenate ions.
In order to more clearly show the technical scheme and the technical effects provided by the present invention, the iron-based complex provided by the embodiment of the present invention and the application thereof are described in detail with specific embodiments below.
Example 1
An iron-based complex, the preparation method of which comprises the following steps: 1.3838mmol of 2-aminoterephthalic acid and 1.3838mmol of FeCl3·6H2Placing O in 30mL of nitrogen-nitrogen dimethyl formamide, carrying out ultrasonic treatment for 5 minutes, stirring for 2 hours, then placing the O in a 50mL reaction kettle, then placing the reaction kettle in a forced air drying oven, carrying out hydrothermal reaction for 20 hours at 120 ℃, taking out suspension in the reaction kettle after the temperature in the forced air drying oven is reduced to room temperature, carrying out centrifugal separation, respectively washing solids obtained by solid-liquid separation for multiple times by using nitrogen-nitrogen dimethyl formamide and ethanol, and finally placing the solids in a freeze drying device for freeze drying for 48 hours, thereby obtaining the iron-based complex.
Specifically, the following morphology and performance tests were performed on the iron-based complex provided in example 1 of the present invention:
(1) the shape of the iron-based complex provided by the embodiment 1 of the invention is observed, so that a scanning electron microscope schematic diagram and a transmission electron microscope schematic diagram shown in FIG. 1 can be obtained; fig. 1a is a schematic scanning electron microscope of the iron-based complex provided in embodiment 1 of the present invention, and fig. 1b is a schematic transmission electron microscope of the iron-based complex provided in embodiment 1 of the present invention. As can be seen from fig. 1: the iron-based complex provided by the embodiment 1 of the invention has an octahedral structure and a regular shape.
(2) The iron-based complex provided in example 1 of the present invention was detected by an X-ray diffractometer, so that an X-ray diffraction pattern as shown in fig. 2 was obtained. As can be seen from fig. 2: the product obtained in example 1 of the invention is indeed an iron-based complex.
(3) Preparing 100ml of arsenate solution with the concentration of 0.1 mu mol/L, 0.5 mu mol/L, 1 mu mol/L, 5 mu mol/L, 10 mu mol/L, 20 mu mol/L, 30 mu mol/L, 40 mu mol/L and 50 mu mol/L respectively, adjusting the pH to 6, then adding 5mg of the iron-based complex provided by the embodiment 1 of the invention respectively, stirring for 10min after 5min of ultrasonic treatment, and detecting the fluorescence intensity of the arsenate solution with each concentration by using a fluorescence spectrometer, thereby obtaining the fluorescence intensity schematic diagram shown in FIG. 3. As can be seen from fig. 3: the iron-based complex provided by the embodiment 1 of the invention is used for carrying out arsenate ion concentration fluorescence detection on a water body with arsenate concentration of 0.1-50 mu mol/L, the fluorescence intensity and the arsenate concentration present a good linear relation, and the fluorescence intensity presents a linear enhancement trend along with the increase of the arsenate ion concentration in the water body; from the fluorescence intensity and the arsenate ion concentration, the detection limit of the iron-based complex provided by the example 1 of the invention can be calculated to be 56nmol/L (4.2ppb) which is lower than the concentration (10ppb) specified by the world health organization.
(4) 17 portions of arsenate solution with the concentration of 6.6 mu mol/L are prepared, and 33 mu mol/L nitrate (the positive ion of the nitrate is Mg)2+、Al3+、Bi3+、Ag+、Cu2+、Co2+、Zn2+、Ni2+、Pb2+、Cr3+) And 33. mu. mol/L of a sodium salt (the anion of the sodium salt is Ac)-、SO4 2-、HCO3 -、CO3 2-、NO3 -、Cl、Br-) Each part of the mixed solution is 100ml, the pH value is adjusted to 6, 5mg of the iron-based complex provided by the embodiment 1 of the invention is added respectively, the mixture is stirred for 10min after being subjected to ultrasonic treatment for 5min, and the fluorescence intensity of each part of the mixed solution is detected by a fluorescence spectrometer respectively, so that the fluorescence property schematic diagram shown in figure 4 can be obtained. As can be seen from fig. 4: in a water body with other cations or anions, the iron-based complex provided by the embodiment 1 of the invention can better realize selective detection of arsenate ions in the water body.
(5) 25ml of arsenate solution with the concentration of 1ppm, 5ppm, 10ppm, 20ppm, 30ppm, 40ppm, 50ppm, 80ppm, 100ppm, 130ppm, 150ppm, 180ppm, 200ppm and 250ppm is prepared, the pH value is adjusted to 6, then 5mg of the iron-based complex provided by the embodiment 1 of the invention is added respectively, after ultrasonic treatment is carried out for 5min, the mixture is continuously stirred for 24 hours at 25 ℃, then part of the liquid is removed from each mixed solution and centrifuged, and passes through a 0.22 mu m filter membrane, the filtrate is collected and marked, and finally, the arsenate ion concentration of each marked filtrate is detected by adopting an inductively coupled plasma mass spectrometer respectively, so that the schematic diagram of the effect of removing the arsenate ions in the water body with different arsenate ion concentrations shown in figure 5 can be obtained. As can be seen from fig. 5: the adsorption capacity of the iron-based complex provided by the embodiment 1 of the invention to the arsenate ions in the water body increases along with the increase of the initial concentration of the arsenate ions, but when the initial concentration of the arsenate ions reaches 100ppm, the adsorption capacity increases smoothly, and the maximum adsorption capacity is 125 mg/g.
(6) Preparing 20ml of 12 parts of 5ppm arsenate solution, adjusting the pH value to 6, then respectively adding 5mg of the iron-based complex provided by the embodiment 1 of the invention, stirring at room temperature, respectively stirring for 1min, 2min, 5min, 10min, 15min, 20min, 30min, 60min, 120min, 180min, 240min and 300min, removing part of liquid from the mixed solution, centrifuging and passing through a 0.22 mu m filter membrane, collecting the filtrate and marking, and finally respectively detecting the arsenate ion concentration of each marked filtrate by adopting an inductive coupling plasma mass spectrometer, so that a schematic diagram of the removal effect of the arsenate ions in the water body at different time points as shown in figure 6 can be obtained. As can be seen from fig. 6: the decline speed of the arsenate ion concentration is very fast in the first 5min, which shows that the iron-based complex provided by the embodiment 1 of the invention has the advantages of fast removal speed and good removal performance; meanwhile, the iron-based complex provided by the embodiment 1 of the invention completely removes the arsenate ions within 3 hours of adsorption, which shows that the iron-based complex provided by the embodiment 1 of the invention has higher removal efficiency on the arsenate ions in the water body.
In conclusion, the embodiment of the invention can not only rapidly detect the concentration of the arsenate ions in the water body and has high detection sensitivity, but also effectively remove the arsenate ions in the water body.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (3)
1. The application of the iron-based complex is characterized in that the iron-based complex is used for detecting the concentration of arsenate ions in a water body or removing the arsenate ions in the water body;
the preparation method of the iron-based complex comprises the following steps: with 2-aminoterephthalic acid and FeCl3·6H2O as raw material, N-dimethyl formamide as solvent, 1.3838mmol FeCl per 1.3838mmol 2-amino terephthalic acid3·6H2Ratio of O to 30mL of Nitrogen-Nitrogen dimethylformamide 2-amino terephthalic acid and FeCl3·6H2Dissolving O in N-N dimethylformamide, then placing the mixture in an environment of 120 ℃ for hydrothermal reaction for 20-24 hours, then carrying out solid-liquid separation, cleaning the solid obtained by the solid-liquid separation, and carrying out freeze drying for 48 hours to obtain the iron-based complex.
2. The application of the iron-based complex as claimed in claim 1, wherein the detection range of the concentration of arsenate ions in the water body per 5mg of the iron-based complex is 0.1-50 μmol/L.
3. The application of the iron-based complex as claimed in claim 1, wherein the dosage of the iron-based complex is 0.2g/L, the pH value of the water body is controlled at 6, and the treatment time is controlled at 24 hours when arsenate ions in the water body are removed.
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