CN111705364B - Preparation method and product of luminescent crystal material for high-sensitivity water-phase detection of 2,4, 6-trinitrophenol - Google Patents

Preparation method and product of luminescent crystal material for high-sensitivity water-phase detection of 2,4, 6-trinitrophenol Download PDF

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CN111705364B
CN111705364B CN202010616224.0A CN202010616224A CN111705364B CN 111705364 B CN111705364 B CN 111705364B CN 202010616224 A CN202010616224 A CN 202010616224A CN 111705364 B CN111705364 B CN 111705364B
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张金方
邱晴霞
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Abstract

The invention discloses a preparation method and a product of a luminescent crystal material of 2,4, 6-trinitrophenol by high-sensitivity water-phase detection, wherein zinc nitrate, 1, 4-phthalic acid and 3,3 ': 5 ', 3 ' -terpyridine are added into an aqueous solution and stirred to prepare a stable suspension, the suspension is placed into a closed reaction kettle for heating reaction, then the temperature is slowly reduced to the room temperature, and the product is filtered, washed and dried to obtain the luminescent crystal material; the invention has the advantages that: obtaining a luminescent crystal material [ Zn ] of 2,4, 6-trinitrophenol by high-sensitivity aqueous phase detection2(L)(BDC)2(H2O)]n。

Description

Preparation method and product of luminescent crystal material for high-sensitivity water-phase detection of 2,4, 6-trinitrophenol
Technical Field
The invention belongs to the technical field of luminescent crystal materials, and particularly relates to a preparation method and a product of a luminescent crystal material for high-sensitivity water-phase detection of 2,4, 6-trinitrophenol.
Background
With the wide application of explosive materials in the industrial field, the hazards to the environment, human health and homeland security are paid much attention, and how to detect these explosives efficiently and reliably has become a hot spot of current research. As a main explosive, 2,4, 6-trinitrophenol is widely applied to industries such as fireworks, dyes, leather and the like, not only causes soil and water system pollution, but also influences human health and causes symptoms such as vomiting, nervous system injury and the like.
Therefore, real-time monitoring of 2,4, 6-trinitrophenol is of great significance for protecting the environment and human health. Luminescent crystalline materials have been used to detect 2,4, 6-trinitrophenol due to their high sensitivity and selectivity in detection applications. The stability of the water phase is a key attribute of the material in practical application, however, most of the luminescent crystal materials reported in the early period are sensitive to water, and the instability of the water phase limits the practical application of the luminescent crystal materials, so that the preparation of the luminescent crystal materials with stable water phase for detecting 2,4, 6-trinitrophenol is more practical.
Disclosure of Invention
This section is for the purpose of summarizing some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. In this section, as well as in the abstract and the title of the invention of this application, simplifications or omissions may be made to avoid obscuring the purpose of the section, the abstract and the title, and such simplifications or omissions are not intended to limit the scope of the invention.
The present invention has been made keeping in mind the above and/or other problems occurring in the prior art.
Therefore, the invention aims to overcome the defects in the prior art and provide a preparation method of a luminescent crystal material for high-sensitivity water-phase detection of 2,4, 6-trinitrophenol.
In order to solve the technical problems, the invention provides the following technical scheme: a method for preparing luminescent crystal material of 2,4, 6-trinitrophenol by high-sensitivity water phase detection comprises adding zinc nitrate, 1, 4-phthalic acid and 3,3 ' 5 ', 3 ' -tripyridine into water solution, stirring to obtain stable suspension; placing the prepared suspension into a closed reaction kettle for heating reaction, slowly cooling to room temperature, filtering, washing and drying the product to obtain the luminescent crystal material [ Zn ]2(L)(BDC)2(H2O)]n(ii) a Wherein the molar ratio of the zinc nitrate, the 1, 4-phthalic acid and the 3,3 ': 5 ', 3 ' -tripyridine is 1: 0.25-1: 0.05-1.
As a preferred scheme of the preparation method of the high-sensitivity water-phase detection 2,4, 6-trinitrophenol luminescent crystal material, the method comprises the following steps: adding zinc nitrate, 1, 4-phthalic acid and 3,3 ', 5 ', 3 ' -tripyridine into an aqueous solution, and stirring, wherein the volume range of the water solvent required by adding 0.2mmol of zinc nitrate is 6-10 mL.
As a preferred scheme of the preparation method of the high-sensitivity water-phase detection 2,4, 6-trinitrophenol luminescent crystal material, the method comprises the following steps: and placing the prepared suspension into a closed reaction kettle for heating reaction, wherein the heating reaction temperature is 140-180 ℃.
As a preferred scheme of the preparation method of the high-sensitivity water-phase detection 2,4, 6-trinitrophenol luminescent crystal material, the method comprises the following steps: and heating for reaction for 48-82 h.
As a preferred scheme of the preparation method of the high-sensitivity water-phase detection 2,4, 6-trinitrophenol luminescent crystal material, the method comprises the following steps: and slowly cooling to room temperature, wherein the reaction cooling rate is 2-7 ℃/h.
As a preferred scheme of the preparation method of the high-sensitivity water-phase detection 2,4, 6-trinitrophenol luminescent crystal material, the method comprises the following steps: adding zinc nitrate, 1, 4-phthalic acid and 3,3 ', 5 ', 3 ' -tripyridine into an aqueous solution, and stirring at a speed of 500-800 r/min for 30-60 min.
As a preferred scheme of the preparation method of the high-sensitivity water-phase detection 2,4, 6-trinitrophenol luminescent crystal material, the method comprises the following steps: the molar ratio of the zinc nitrate, the 1, 4-phthalic acid and the 3,3 ': 5 ', 3 ' -tripyridine is 0.2:0.1: 0.05.
As a preferred scheme of the preparation method of the high-sensitivity water-phase detection 2,4, 6-trinitrophenol luminescent crystal material, the method comprises the following steps: the luminescent crystal material [ Zn ] is obtained after the drying2(L)(BDC)2(H2O)]nAnd drying at the temperature of 30-40 ℃ for 12-14 h.
It is another object of the present invention to overcome the deficiencies of the prior art and to provide a luminescent crystal material for high-sensitivity aqueous phase detection of 2,4, 6-trinitrophenol.
As a preferred scheme of the high-sensitivity water-phase detection luminescent crystal material of the 2,4, 6-trinitrophenol, the invention comprises the following steps: the luminescent crystal material is [ Zn ]2(L)(BDC)2(H2O)]nThe fluorescent probe has strong luminescence and higher water stability, can detect the 2,4, 6-trinitrophenol in water with high sensitivity, and shows fluorescence quenching.
The invention has the beneficial effects that:
(1) the invention provides a preparation method of a luminescent crystal material for high-sensitivity water-phase detection of 2,4, 6-trinitrophenol, which adopts a hydrothermal synthesis method, and has simple synthetic route and easy control; the synthetic raw materials are simple to prepare; high purity of crystal and high yield.
(2) The material prepared by the invention can be used for high-sensitivity fluorescence detection of 2,4, 6-trinitrophenol in water, and has good chemical and optical stability.
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 will be 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 these drawings without inventive exercise. Wherein:
FIG. 1 shows a crystalline material [ Zn ] obtained in example 1 of the present invention2(L)(BDC)2(H2O)]nA three-dimensional structure diagram (some atoms are omitted).
FIG. 2 shows a crystalline material [ Zn ] prepared in example 1 of the present invention2(L)(BDC)2(H2O)]nPowder X-ray diffraction pattern of (1).
FIG. 3 shows a crystalline material [ Zn ] obtained in example 1 of the present invention2(L)(BDC)2(H2O)]nTo which different volumes of 2,4, 6-trinitrophenol aqueous solution (1 millimole per liter) were added.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention more comprehensible, specific embodiments thereof are described in detail below with reference to examples of the specification.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
Furthermore, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
The invention comprises the following raw materials: 3,3 ', 5 ', 3 ' -tripyridine, which is synthesized according to published documents, particularly: T.H.Chuang, Y.C.Chen, S.Pola, J.org.chem.2010,75, 6625-.
Example 1
The invention relates to a luminescent crystal material [ Zn ] for high-sensitivity aqueous phase detection of 2,4, 6-trinitrophenol2(L)(BDC)2(H2O)]nThe preparation method comprises the following steps:
(1) step one, adding 0.2mmol of zinc nitrate, 0.1mmol of 1, 4-phthalic acid and 0.05mmol of 3,3 ', 5 ', 3 ' -tripyridine into 6mL of water, and stirring to obtain a stable suspension, wherein the stirring speed is 500r/min, and the stirring time is 60 min;
(2) and step two, placing the suspension prepared in the step one in a closed reaction kettle, heating to 140 ℃, reacting for 72 hours, slowly cooling to room temperature at the rate of 2 ℃ per hour, filtering, washing, and drying at 40 ℃ for 14 hours to obtain the crystal material, wherein the yield reaches 55.2%.
FIG. 1 shows a crystalline material [ Zn ] obtained in example 1 of the present invention2(L)(BDC)2(H2O)]nThree-dimensional structure of (part of atoms omitted)
Prepared crystalline material [ Zn ]2(L)(BDC)2(H2O)]nThe powder X-ray diffraction pattern of (A) is shown in FIG. 2. As can be seen from FIG. 2, the crystalline material [ Zn ] prepared by the present invention2(L)(BDC)2(H2O)]nThe powder X-ray diffraction pattern is basically consistent with the X-ray diffraction pattern calculated by theory, which shows that the crystal material prepared by the invention has high purity. The X-ray diffraction pattern of the prepared crystal material after being soaked in water for one week is basically consistent with the X-ray diffraction pattern calculated theoretically,thus, the prepared crystal has good stability in water.
(3) Detecting the detection performance of 2,4, 6-trinitrophenol: the prepared crystalline material (1 mg) was dispersed in 3 ml of water, and various volumes of aqueous solutions (1 mmol per liter) containing 2,4, 6-trinitrophenol were added thereto, and the fluorescence intensities thereof were measured under excitation light of 320nm, respectively.
As a result, as shown in FIG. 3, it can be seen from FIG. 3 that the fluorescence intensity of the aqueous suspension of the crystals was measured at an excitation wavelength of 320nm (55035), and then 1mmol/L of an aqueous 2,4, 6-trinitrophenol solution was gradually added dropwise thereto, the luminescence intensity was gradually decreased as the amount of 2,4, 6-trinitrophenol was increased, and when 260uL of 2,4, 6-trinitrophenol aqueous solution was added, the fluorescence intensity was remarkably decreased (9164), and the quenching efficiency was 83.86%, whereby it can be seen that the material can detect 2,4, 6-trinitrophenol in a highly sensitive aqueous phase.
Example 2
The invention relates to a luminescent crystal material [ Zn ] for high-sensitivity aqueous phase detection of 2,4, 6-trinitrophenol2(L)(BDC)2(H2O)]nThe preparation method comprises the following steps:
step one, adding 0.2mmol of zinc nitrate, 0.1mmol of 1, 4-phthalic acid and 0.05mmol of 3,3 ', 5 ', 3 ' -tripyridine into 6mL of water, and stirring to obtain a stable suspension, wherein the stirring speed is 500r/min, and the stirring time is 60 min;
and step two, placing the suspension prepared in the step one in a closed reaction kettle, heating to 150 ℃, reacting for 72 hours, slowly cooling to room temperature at the rate of 2 ℃ per hour, filtering, washing, and drying at 40 ℃ for 14 hours to obtain the crystal material.
Detecting the detection performance of 2,4, 6-trinitrophenol: the prepared crystalline material (1 mg) was dispersed in 3 ml of water, and various volumes of aqueous solutions (1 mmol per liter) containing 2,4, 6-trinitrophenol were added thereto, and the fluorescence intensities thereof were measured under excitation light of 320nm, respectively. As can be seen, the luminous intensity of the material is gradually reduced along with the increase of the amount of the 2,4, 6-trinitrophenol, and the material can detect the 2,4, 6-trinitrophenol in a high-sensitivity water phase.
Example 3
The invention relates to a luminescent crystal material [ Zn ] for high-sensitivity aqueous phase detection of 2,4, 6-trinitrophenol2(L)(BDC)2(H2O)]nThe preparation method comprises the following steps:
step one, adding 0.2mmol of zinc nitrate, 0.1mmol of 1, 4-phthalic acid and 0.05mmol of 3,3 ', 5 ', 3 ' -tripyridine into 6mL of water, and stirring to obtain a stable suspension, wherein the stirring speed is 500r/min, and the stirring time is 60 min;
and step two, placing the suspension prepared in the step one in a closed reaction kettle, heating to 150 ℃, reacting for 72 hours, slowly cooling to room temperature at the rate of 5 ℃ per hour, filtering, washing, and drying at 40 ℃ for 14 hours to obtain the crystal material.
Detecting the detection performance of 2,4, 6-trinitrophenol: the prepared crystalline material (1 mg) was dispersed in 3 ml of water, and various volumes of aqueous solutions (1 mmol per liter) containing 2,4, 6-trinitrophenol were added thereto, and the fluorescence intensities thereof were measured under excitation light of 320nm, respectively. As can be seen, the luminous intensity of the material is gradually reduced along with the increase of the amount of the 2,4, 6-trinitrophenol, and the material can detect the 2,4, 6-trinitrophenol in a high-sensitivity water phase.
Example 4
The invention relates to a luminescent crystal material [ Zn ] for high-sensitivity aqueous phase detection of 2,4, 6-trinitrophenol2(L)(BDC)2(H2O)]nThe preparation method comprises the following steps:
step one, adding 0.2mmol of zinc nitrate, 0.1mmol of 1, 4-phthalic acid and 0.05mmol of 3,3 ', 5 ', 3 ' -tripyridine into 6mL of water, and stirring to obtain a stable suspension, wherein the stirring speed is 500r/min, and the stirring time is 60 min;
and step two, placing the suspension prepared in the step one in a closed reaction kettle, heating to 160 ℃, reacting for 72 hours, slowly cooling to room temperature at the rate of 5 ℃ per hour, filtering, washing, and drying at 40 ℃ for 14 hours to obtain the crystal material.
Detecting the detection performance of 2,4, 6-trinitrophenol: the prepared crystalline material (1 mg) was dispersed in 3 ml of water, and various volumes of aqueous solutions (1 mmol per liter) containing 2,4, 6-trinitrophenol were added thereto, and the fluorescence intensities thereof were measured under excitation light of 320nm, respectively. As can be seen, the luminous intensity of the material is gradually reduced along with the increase of the amount of the 2,4, 6-trinitrophenol, and the material can detect the 2,4, 6-trinitrophenol in a high-sensitivity water phase.
Example 5
The invention relates to a luminescent crystal material [ Zn ] for high-sensitivity aqueous phase detection of 2,4, 6-trinitrophenol2(L)(BDC)2(H2O)]nThe preparation method comprises the following steps:
step one, adding 0.2mmol of zinc nitrate, 0.1mmol of 1, 4-phthalic acid and 0.05mmol of 3,3 ', 5 ', 3 ' -tripyridine into 6mL of water, and stirring to obtain a stable suspension, wherein the stirring speed is 500r/min, and the stirring time is 60 min;
and step two, placing the suspension prepared in the step one in a closed reaction kettle, heating to 160 ℃, reacting for 72 hours, slowly cooling to room temperature at the rate of 2 ℃ per hour, filtering, washing, and drying at 40 ℃ for 14 hours to obtain the crystal material.
Detecting the detection performance of 2,4, 6-trinitrophenol: the prepared crystalline material (1 mg) was dispersed in 3 ml of water, and various volumes of aqueous solutions (1 mmol per liter) containing 2,4, 6-trinitrophenol were added thereto, and the fluorescence intensities thereof were measured under excitation light of 320nm, respectively. As can be seen, the luminous intensity of the material is gradually reduced along with the increase of the amount of the 2,4, 6-trinitrophenol, and the material can detect the 2,4, 6-trinitrophenol in a high-sensitivity water phase.
Example 6
The invention relates to a luminescent crystal material [ Zn ] for high-sensitivity aqueous phase detection of 2,4, 6-trinitrophenol2(L)(BDC)2(H2O)]nThe preparation method comprises the following steps:
(1) step one, adding 0.1mmol of zinc nitrate, 0.1mmol of 1, 4-phthalic acid and 0.05mmol of 3,3 ', 5 ', 3 ' -tripyridine into 6mL of water, and stirring to obtain a stable suspension, wherein the stirring speed is 500r/min, and the stirring time is 60 min;
(2) and step two, placing the suspension prepared in the step one in a closed reaction kettle, heating to 140 ℃, reacting for 72 hours, slowly cooling to room temperature at the rate of 2 ℃ per hour, filtering, washing, and drying at 40 ℃ for 14 hours to obtain the crystal material.
Detecting the detection performance of 2,4, 6-trinitrophenol: the prepared crystalline material (1 mg) was dispersed in 3 ml of water, and various volumes of aqueous solutions (1 mmol per liter) containing 2,4, 6-trinitrophenol were added thereto, and the fluorescence intensities thereof were measured under excitation light of 320nm, respectively. As can be seen, the luminous intensity of the material is gradually reduced along with the increase of the amount of the 2,4, 6-trinitrophenol, and the material can detect the 2,4, 6-trinitrophenol in a high-sensitivity water phase.
Example 7
The invention relates to a luminescent crystal material [ Zn ] for high-sensitivity aqueous phase detection of 2,4, 6-trinitrophenol2(L)(BDC)2(H2O)]nThe preparation method comprises the following steps:
(1) step one, adding 0.3mmol of zinc nitrate, 0.1mmol of 1, 4-phthalic acid and 0.05mmol of 3,3 ', 5 ', 3 ' -tripyridine into 6mL of water, and stirring to obtain a stable suspension, wherein the stirring speed is 500r/min, and the stirring time is 60 min;
(2) and step two, placing the suspension prepared in the step one in a closed reaction kettle, heating to 140 ℃, reacting for 72 hours, slowly cooling to room temperature at the rate of 2 ℃ per hour, filtering, washing, and drying at 40 ℃ for 14 hours to obtain the crystal material.
Detecting the detection performance of 2,4, 6-trinitrophenol: the prepared crystalline material (1 mg) was dispersed in 3 ml of water, and various volumes of aqueous solutions (1 mmol per liter) containing 2,4, 6-trinitrophenol were added thereto, and the fluorescence intensities thereof were measured under excitation light of 320nm, respectively. As can be seen, the luminous intensity of the material is gradually reduced along with the increase of the amount of the 2,4, 6-trinitrophenol, and the material can detect the 2,4, 6-trinitrophenol in a high-sensitivity water phase.
Example 8
The invention relates to a luminescent crystal material [ Zn ] for high-sensitivity aqueous phase detection of 2,4, 6-trinitrophenol2(L)(BDC)2(H2O)]nThe preparation method comprises the following steps:
(1) step one, adding 0.2mmol of zinc nitrate, 0.2mmol of 1, 4-phthalic acid and 0.05mmol of 3,3 ', 5 ', 3 ' -tripyridine into 6mL of water, and stirring to obtain a stable suspension, wherein the stirring speed is 500r/min, and the stirring time is 60 min;
(2) and step two, placing the suspension prepared in the step one in a closed reaction kettle, heating to 140 ℃, reacting for 72 hours, slowly cooling to room temperature at the rate of 2 ℃ per hour, filtering, washing, and drying at 40 ℃ for 14 hours to obtain the crystal material.
Detecting the detection performance of 2,4, 6-trinitrophenol: the prepared crystalline material (1 mg) was dispersed in 3 ml of water, and various volumes of aqueous solutions (1 mmol per liter) containing 2,4, 6-trinitrophenol were added thereto, and the fluorescence intensities thereof were measured under excitation light of 320nm, respectively. As can be seen, the luminous intensity of the material is gradually reduced along with the increase of the amount of the 2,4, 6-trinitrophenol, and the material can detect the 2,4, 6-trinitrophenol in a high-sensitivity water phase.
Example 9
The invention relates to a luminescent crystal material [ Zn ] for high-sensitivity aqueous phase detection of 2,4, 6-trinitrophenol2(L)(BDC)2(H2O)]nThe preparation method comprises the following steps:
(1) step one, adding 0.2mmol of zinc nitrate, 0.05mmol of 1, 4-phthalic acid and 0.05mmol of 3,3 ', 5 ', 3 ' -tripyridine into 6mL of water, and stirring to obtain a stable suspension, wherein the stirring speed is 500r/min, and the stirring time is 60 min;
(2) and step two, placing the suspension prepared in the step one in a closed reaction kettle, heating to 140 ℃, reacting for 72 hours, slowly cooling to room temperature at the rate of 2 ℃ per hour, filtering, washing, and drying at 40 ℃ for 14 hours to obtain the crystal material.
Detecting the detection performance of 2,4, 6-trinitrophenol: the prepared crystalline material (1 mg) was dispersed in 3 ml of water, and various volumes of aqueous solutions (1 mmol per liter) containing 2,4, 6-trinitrophenol were added thereto, and the fluorescence intensities thereof were measured under excitation light of 320nm, respectively. As can be seen, the luminous intensity of the material is gradually reduced along with the increase of the amount of the 2,4, 6-trinitrophenol, and the material can detect the 2,4, 6-trinitrophenol in a high-sensitivity water phase.
The yield of the crystalline material obtained in the present invention was calculated based on the amount of zinc ions added.
The yields of crystalline materials obtained in examples 6 to 9 are shown in Table 1.
TABLE 1
Figure GDA0003020245390000081
As can be seen from Table 1, when the ratio of the reactants added is not proper, less crystals are precipitated and the yield is low. When the molar ratio of the reaction starting materials is not optimal, the yields of crystalline material differ significantly; but are all high purity crystalline materials. The inventor further studies and finds that when the reaction starting materials are in the optimal molar ratio, the yield and the purity of the crystal materials are basically the same; different reaction temperatures, times and cooling rates can lead to different crystal sizes of the crystal materials, but the quality of the materials cannot be caused.
Crystalline material [ Zn ] prepared by the invention2(L)(BDC)2(H2O)]nThe powder X-ray diffraction pattern is basically consistent with the X-ray diffraction pattern calculated by theory, which shows that the crystal material prepared by the invention has high purity. The X-ray diffraction pattern of the prepared crystal material after being soaked in water for one week is basically consistent with the X-ray diffraction pattern calculated by theory, which shows that the prepared crystal has good stability in water.
Crystalline material [ Zn ] produced by the invention2(L)(BDC)2(H2O)]nThe fluorescence intensity of the aqueous suspension of the crystals was measured at an excitation wavelength of 320nm (55035), and then 1mmol/L of an aqueous 2,4, 6-trinitrophenol solution was gradually added dropwise thereto, the luminescence intensity was gradually decreased as the amount of 2,4, 6-trinitrophenol was increased, and when 260uL of an aqueous 2,4, 6-trinitrophenol solution was added, the fluorescence intensity was significantly decreased (9164) and the quenching efficiency was 83.86%, and the material was capable of highly sensitive aqueous phase detection of 2,4, 6-trinitrophenol.
The invention provides a preparation method of a luminescent crystal material for high-sensitivity water-phase detection of 2,4, 6-trinitrophenol, which adopts a hydrothermal synthesis method, and has simple synthetic route and easy control; the synthetic raw materials are simple to prepare; high purity of crystal and high yield. The material prepared by the invention can be used for high-sensitivity fluorescence detection of 2,4, 6-trinitrophenol in water, and has good chemical and optical stability.
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.

Claims (8)

1. A preparation method of a luminescent crystal material for high-sensitivity water-phase detection of 2,4, 6-trinitrophenol is characterized by comprising the following steps: comprises the steps of (a) preparing a mixture of a plurality of raw materials,
adding zinc nitrate, 1, 4-phthalic acid and 3,3 '5', 3 '' -tripyridine into the aqueous solution, and stirring to obtain a stable suspension;
placing the prepared suspension into a closed reaction kettle for heating reaction, slowly cooling to room temperature, filtering, washing and drying the product to obtain the luminescent crystal material [ Zn ]2(L)(BDC)2(H2O)]n(ii) a Wherein L is 3,3 ', 5', 3 '' -tripyridine;
the molar ratio of the zinc nitrate, 1, 4-phthalic acid and 3,3 ': 5', 3 '' -tripyridine is 0.2:0.1: 0.05.
2. The method for preparing the luminescent crystal material of 2,4, 6-trinitrophenol by the high-sensitivity aqueous phase detection as claimed in claim 1, wherein the method comprises the following steps: the zinc nitrate, the 1, 4-phthalic acid and the 3,3 ': 5', 3 '' -tripyridine are added into the aqueous solution and stirred, wherein the volume range of the water solvent required by adding 0.2mmol of zinc nitrate is 6-10 mL.
3. The method for preparing the luminescent crystal material of 2,4, 6-trinitrophenol by the high-sensitivity aqueous phase detection as claimed in claim 1, wherein the method comprises the following steps: and placing the prepared suspension into a closed reaction kettle for heating reaction, wherein the heating reaction temperature is 140-180 ℃.
4. The method for preparing the luminescent crystal material of 2,4, 6-trinitrophenol by the high-sensitivity aqueous phase detection as claimed in claim 3, wherein the method comprises the following steps: and heating for reaction for 48-82 h.
5. The method for preparing the luminescent crystal material of 2,4, 6-trinitrophenol by the high-sensitivity aqueous phase detection as claimed in claim 1, wherein the method comprises the following steps: and slowly cooling to room temperature, wherein the reaction cooling rate is 2-7 ℃/h.
6. The method for preparing the luminescent crystal material of 2,4, 6-trinitrophenol by the high-sensitivity aqueous phase detection as claimed in claim 1, wherein the method comprises the following steps: the zinc nitrate, the 1, 4-phthalic acid and the 3,3 ': 5', 3 '' -tripyridine are added into the water solution and stirred, wherein the stirring speed is 500-800 r/min, and the stirring time is 30-60 min.
7. The method for preparing the luminescent crystal material of 2,4, 6-trinitrophenol by the high-sensitivity aqueous phase detection as claimed in claim 1, wherein the method comprises the following steps: the luminescent crystal material [ Zn ] is obtained after the drying2(L)(BDC)2(H2O)]nAnd drying at the temperature of 30-40 ℃ for 12-14 h.
8. A product prepared by the preparation method of the luminescent crystal material for high-sensitivity water-phase detection of 2,4, 6-trinitrophenol as claimed in any one of claims 1 to 7.
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CN108034990A (en) * 2017-12-08 2018-05-15 江南大学 Can highly sensitive detection 2,4,6- trinitrophenols luminescent crystal material preparation
CN109517185A (en) * 2018-11-05 2019-03-26 合肥学院 A kind of rare earth metal-organic framework material [Dy2(BDC)3(H2O)4]nPreparation method and application
CN110655529A (en) * 2019-10-21 2020-01-07 江南大学 Preparation of luminescent crystal material for rapidly and highly sensitively detecting high manganese acid radical ions

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* Cited by examiner, † Cited by third party
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CN108034990A (en) * 2017-12-08 2018-05-15 江南大学 Can highly sensitive detection 2,4,6- trinitrophenols luminescent crystal material preparation
CN109517185A (en) * 2018-11-05 2019-03-26 合肥学院 A kind of rare earth metal-organic framework material [Dy2(BDC)3(H2O)4]nPreparation method and application
CN110655529A (en) * 2019-10-21 2020-01-07 江南大学 Preparation of luminescent crystal material for rapidly and highly sensitively detecting high manganese acid radical ions

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