CN112371096A - Preparation method and application of organic-inorganic composite material for removing multiple heavy metals in water - Google Patents

Preparation method and application of organic-inorganic composite material for removing multiple heavy metals in water Download PDF

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CN112371096A
CN112371096A CN202011216483.0A CN202011216483A CN112371096A CN 112371096 A CN112371096 A CN 112371096A CN 202011216483 A CN202011216483 A CN 202011216483A CN 112371096 A CN112371096 A CN 112371096A
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powder
tank
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殷娇
朱慧
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Xinjiang Technical Institute of Physics and Chemistry of CAS
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Xinjiang Technical Institute of Physics and Chemistry of CAS
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Abstract

The invention provides a preparation method and application of an organic-inorganic composite material for removing multiple heavy metals in water, the method relates to a device which comprises a dry powder mixing tank, a powder conveying pipe, a solid-liquid stirring tank, a stirring screw, a solution preparation tank, a solution conveying pipe, a solution spraying pipe, a solution nozzle, a gamma ray radiation source, a discharge port, a turbid liquid collecting tank, a stirrer, a bracket, a moving wheel, a turbid liquid conveying pipe, a spray dryer, a powder collector, a continuous carbonization furnace, a powder stirring tank and a storage tank, wherein the raw materials comprise modified potassium feldspar, modified vermiculite, high-index surface titanium dioxide, sodium titanate, boron nitride, carbon nitride, polyethylene glycol and water, the turbid liquid obtained after mixing the raw materials is subjected to spray drying after being radiated by gamma rays, spherical powder materials are obtained after spray drying, and then the powder materials are roasted in an inert atmosphere at a low temperature, then the organic-inorganic composite material with abundant lattice defects and used for removing various heavy metals in water is obtained by gamma ray radiation.

Description

Preparation method and application of organic-inorganic composite material for removing multiple heavy metals in water
Technical Field
The invention relates to a preparation method and application of an organic-inorganic composite material for removing multiple heavy metal ions in water simultaneously.
Background
Heavy metal ion pollution is an important environmental pollutant in water, and mainly comprises heavy metal ions such as copper, nickel, cobalt, lead, cadmium, mercury, chromium and the like. The long-term intake of water source or food containing heavy metal ions seriously threatens the health of human bodies, and causes teratogenesis, carcinogenesis and mutation. At present, the main methods for removing heavy metal ions in water bodies include precipitation methods, ion exchange methods, electrochemical reduction methods, membrane filtration methods, evaporation and solidification methods, adsorption methods and the like, wherein the adsorption methods are widely applied due to the advantages of high efficiency, low cost, cyclic utilization, environmental protection and the like. The large-scale application of the adsorption method mainly benefits from the high-efficiency adsorption performance of the adsorbent. The existing heavy metal ion adsorbent mainly comprises activated carbon, molecular sieve, ion exchange resin and the like. The adsorbents have the defects of low adsorption capacity, low adsorption speed, low adsorption selectivity and low regeneration efficiency, are difficult to remove various heavy metal ions simultaneously, have low removal rate to the heavy metal ions with low concentration (within 200 ppb) in a water body, and are difficult to reach the emission standard of less than 5 ppb.
Disclosure of Invention
The invention aims to provide a preparation method and application of an organic-inorganic composite material for removing multiple heavy metals in water aiming at the defects of the existing adsorption material, the method relates to a device which comprises a dry powder mixing tank, a first powder conveying pipe, a solid-liquid stirring tank, a first stirring screw, a solution preparation tank, a solution conveying pipe, a solution spraying pipe, a solution nozzle, a gamma ray radiation source, a first discharge port, a suspension collecting tank, a stirrer, a bracket, a moving wheel, a suspension conveying pipe, a spray dryer, a powder collector, a second powder conveying pipe, a continuous carbonization furnace, a second discharge port, a powder stirring tank, a second stirring screw, a third discharge port and a storage tank, wherein the raw materials comprise modified potassium feldspar, modified vermiculite, high index surface titanium dioxide, sodium titanate, boron nitride, carbon nitride, polyethylene glycol and water which are used as raw materials, the suspension is irradiated by gamma rays and then is subjected to spray drying, spray drying to obtain spherical powder material, roasting the powder material in inert atmosphere at low temperature, and radiating with gamma ray to obtain the organic-inorganic composite material with rich lattice defects and capable of removing various heavy metals in water.
The invention relates to a preparation method of an organic-inorganic composite material for removing multiple heavy metal ions in water, which comprises a dry powder mixing tank (1), a first powder conveying pipe (2), a solid-liquid stirring tank (3), a first stirring screw (4), a solution preparation tank (5), a solution conveying pipe (6), a solution spraying pipe (7), a solution nozzle (8), a gamma ray radiation source (9), a first discharge hole (10), a suspension collecting tank (11), a stirrer (12), a support (13), a moving wheel (14), a suspension conveying pipe (15), a spray dryer (16), a powder collector (17), a second powder conveying pipe (18), a continuous carbonization furnace (19), a second discharge hole (20), a powder stirring tank (21), a second stirring screw (22), a third discharge hole (23) and a material storage tank (24), the dry powder mixing tank (1) is connected with a solid-liquid stirring tank (3) through a first powder conveying pipe (2), a first stirring screw (4) is arranged in the solid-liquid stirring tank (3), a solution preparation tank (5) is arranged at the top end of the solid-liquid stirring tank (3), the solution preparation tank (5) is connected with a solution spraying pipe (7) through a solution conveying pipe (6), a plurality of solution nozzles (8) which are arranged evenly are arranged on the solution spraying pipe (7), a first discharge hole (10) is arranged at the bottom of the solid-liquid stirring tank (3), the first discharge hole (10) is connected with a suspension collecting tank (11), a stirrer (12) is arranged in the suspension collecting tank (11), supports (13) of movable wheels (14) are fixed at two ends of the bottom of the solid-liquid stirring tank (3), and the bottom of the suspension collecting tank (11) is connected with a spray dryer (16) through a conveying pipe (15), a powder collector (17) is arranged at the bottom of the spray dryer (16), the powder collector (17) is connected with one end of a continuous carbonization furnace (19) through a second powder conveying pipe (18), the other end of the continuous carbonization furnace (19) is connected with a powder stirring tank (21) through a second discharge hole (20), a second stirring screw (22) is arranged in the powder stirring tank (21), a third discharge hole (23) is arranged at the bottom of the powder stirring tank (21), the third discharge hole (23) is connected with a storage tank (24), and the solid-liquid stirring tank (3) and the powder stirring tank (21) are respectively arranged under a gamma-ray radiation source for stirring; the method takes modified potash feldspar, modified vermiculite, high index surface titanium dioxide, sodium titanate, boron nitride, carbon nitride, polyethylene glycol and water as raw materials, adopts gamma-ray radiation, spray drying, roasting in inert atmosphere and then gamma-ray radiation, and concretely comprises the following steps:
a. respectively mixing modified potash feldspar, modified vermiculite, high index surface titanium dioxide, sodium titanate, boron nitride and carbon nitride in a mass ratio of 0.01-1:0.01-1:0.01-1:0.01-1, and fully stirring to obtain mixed powder;
b. dissolving polyethylene glycol in water according to the mass ratio of 0.01-1:1-10 to obtain a polyethylene glycol aqueous solution, putting the polyethylene glycol aqueous solution into a solution preparation tank (5), transferring the mixed powder obtained in the step a into a solid-liquid stirring tank (3) through a first powder conveying pipe (2), and uniformly spraying the polyethylene glycol aqueous solution in the solution preparation tank (5) into the solid-liquid stirring tank (3) through a solution conveying pipe (6), a solution spraying pipe (7) and a solution nozzle (8) to obtain a suspension, wherein the polyethylene glycol is PEG-200, PEG-400, PEG-600, PEG-800, PEG-1000 or PEG-2000;
c. starting a first stirring screw (4), stirring the suspension liquid in the step b for 1 hour, and then placing a solid-liquid stirring tank (3) under gamma rays (9) for irradiation for 1-5 hours, wherein the radiation dose of the gamma rays is as follows: 0.002 rad/s-1000 rad/s, the first stirring screw (4) in the solid-liquid stirring tank (3) is always opened while the radiation is carried out, the suspension is always in a high-speed stirring state, after the radiation is finished, the suspension in the solid-liquid stirring tank (3) is transferred into a suspension collecting tank (11) through a first discharge port (10), a stirrer (12) arranged in the suspension collecting tank (11) is always opened, and the suspension is always in a high-speed stirring state;
d. the suspension in the suspension collecting tank (11) is transferred into a spray dryer (16) through a suspension conveying pipe (15) for spray drying, the powder after spray drying is transferred into a powder collector (17), then the powder is transferred into a continuous carbonization furnace (19) through a second powder conveying pipe (18), the powder is roasted for 1 to 5 hours at the temperature of between 60 and 300 ℃, the roasted powder is transferred into a powder stirring tank (21) through a second discharge hole (20), the powder stirring tank (21) is placed under gamma rays (9) for irradiation for 1 to 5 hours, and the radiation dose of the gamma rays is as follows: 0.002 rad/s-1000 rad/s, the second stirring screw (22) in the powder stirring tank (21) is always opened while the powder is irradiated, and the powder is always in a high-speed stirring state;
e. after the irradiation is finished, the powder in the powder stirring tank (21) is transferred into a storage tank (24) through a third discharge hole (23), and the organic-inorganic composite material rich in crystal defect structures and with the grain size distribution of 60-200 meshes is obtained.
The organic-inorganic composite material obtained by the method is used for preparing and removing various heavy metal ions such as nickel, cobalt, lead, cadmium, mercury, chromium and arsenic ions.
The invention relates to a preparation method of an organic-inorganic composite material for removing multiple heavy metal ions in water, wherein the modification method of modified potassium feldspar in the method comprises dilute hydrochloric acid treatment and high-temperature roasting, the concentration of hydrochloric acid is 0.01-1%, and the high-temperature roasting temperature is 100-500 ℃;
the modification method of the modified vermiculite comprises the steps of treating by using low-concentration sodium chloride and roasting at high temperature, wherein the concentration of the sodium chloride is 1-10%, and the roasting temperature at high temperature is 100-;
the crystal face of the high-index crystal face titanium dioxide is mainly 201 face, and the proportion of the 201 face is 50-80%;
sodium titanate and boron nitride as nanotubes, carbon nitride (g-C)3N4) Is a nano-sheet with a specific surface area of 50-150m2/g。
The invention relates to a preparation method of an organic-inorganic composite material for removing various heavy metal ions in water, which is characterized in that the microstructure of an adsorbent is regulated and controlled from the action mechanism between the heavy metal ions and the adsorbent, the crystal structure of the adsorbent is regulated and controlled through gamma ray radiation, and vacancies of metal ions and oxygen atoms are generated on the surface and inside of the adsorbent by means of the action of an external field of rays, namely, defects are constructed from different dimensions, so that the adsorption capacity and the adsorption selectivity of the adsorbent on the heavy metal ions are improved. Meanwhile, the spherical powder material with high dispersibility is prepared by means of the regulation and control effect of a spray drying method on the granularity and the micro-morphology of the material.
The organic-inorganic composite material obtained by the method has the removal rate of 99% for heavy metal ions of nickel, cobalt, lead, cadmium, mercury, chromium and arsenic with the low concentration of 100ppb or less, and has the removal rate of more than 96% for heavy metal ions of nickel, cobalt, lead, cadmium, mercury, chromium and arsenic with the high concentration of 500-1000 ppb. The adsorption capacity is as high as 0.8-1 g/g. The preparation method of the composite material is simple, convenient to operate, environment-friendly, safe, free of additional pollutants, good in adsorption performance, high in adsorption speed, recyclable, long in service life, low in energy consumption and suitable for large-scale industrial production.
The nitrogen adsorption and desorption test of the organic-inorganic composite material obtained by the method of the invention shows that: has rich pore structure and larger specific surface area which is as high as 300-400m2The composite material has the advantages that the composite material has obvious characteristic peaks of components such as potassium feldspar, vermiculite, high-index surface titanium dioxide, sodium titanate, boron nitride, polyethylene glycol and the like through ESR, ultraviolet visible diffuse reflection, XRD, infrared and Raman spectrum tests, and ESR and ultraviolet visible diffuse reflection tests show that the composite material has rich defect structures. The composite material has strong adsorption capacity to heavy metal ions, and has the advantages of low cost, rich resources and no toxicity. The adsorbent is applied to the field of prevention and control of heavy metal pollutants in water, the removal rate of the adsorbent on heavy metal ions of nickel, cobalt, lead, cadmium, mercury, chromium and arsenic with the low concentration of 100ppb is up to 99%, the removal rate on heavy metal ions of nickel, cobalt, lead, cadmium, mercury, chromium and arsenic with the high concentration of 500-1000 ppb is up to 96%, and the removal rates of the heavy metal ions are shown in table 1; table 2 shows that the defect structure produced by gamma radiation is a key factor for determining the composite material has high adsorption performance to heavy metal ions, and other materials have no good removal performance instead, which indicates that other materials do not have strong removal function to radioactive metal ions.
Drawings
FIG. 1 is a schematic diagram of the preparation route of the organic-inorganic composite material of the present invention;
FIG. 2 is a high-resolution scanning electron microscope (a) and a transmission electron microscope (b) of the organic-inorganic composite material according to the present invention;
FIG. 3 is a nitrogen adsorption and desorption graph of the organic-inorganic composite material of the present invention, wherein (a) a nitrogen adsorption curve; (b) pore size distribution curve;
FIG. 4 shows an ESR spectrum (a) and a UV-visible diffuse reflectance spectrum (b) of the organic-inorganic composite material according to the present invention;
FIG. 5 is a view showing an apparatus for producing an organic-inorganic composite material according to the present invention.
Detailed Description
For further understanding of the present invention, the present invention will be described in detail with reference to the following examples, but the present invention is not limited to the examples.
Example 1
The invention relates to a preparation method of an organic-inorganic composite material for removing multiple heavy metal ions in water, which comprises a dry powder mixing tank 1, a first powder conveying pipe 2, a solid-liquid stirring tank 3, a first stirring screw 4, a solution preparation tank 5, a solution conveying pipe 6, a solution spraying pipe 7, a solution nozzle 8, a gamma-ray radiation source 9, a first discharge port 10, a suspension collecting tank 11, a stirrer 12, a bracket 13, a moving wheel 14, a suspension conveying pipe 15, a spray dryer 16, a powder collector 17, a second powder conveying pipe 18, a continuous carbonization furnace 19, a second discharge port 20, a powder stirring tank 21, a second stirring screw 22, a third discharge port 23 and a material storage tank 24, wherein the dry powder mixing tank 1 is connected with the solid-liquid stirring tank 3 through the first powder conveying pipe 2, the first stirring screw 4 is arranged in the solid-liquid stirring tank 3, the top of the solid-liquid stirring tank 3 is provided with a solution preparation tank 5, the solution preparation tank 5 is connected with a solution spraying pipe 7 through a solution conveying pipe 6, the solution spraying pipe 7 is provided with a plurality of solution nozzles 8 which are arranged equally, the bottom of the solid-liquid stirring tank 3 is provided with a first discharge hole 10, the first discharge hole 10 is connected with a suspension collecting tank 11, a stirrer 12 is arranged in the suspension collecting tank 11, two ends of the bottom of the solid-liquid stirring tank 3 are provided with a support 13 with movable wheels 14, the bottom of the suspension collecting tank 11 is connected with a spray dryer 16 through a suspension conveying pipe 15, the bottom of the spray dryer 16 is provided with a powder collector 17, the powder collector 17 is connected with one end of a continuous carbonization furnace 19 through a second powder conveying pipe 18, the other end of the continuous carbonization furnace 19 is connected with a powder stirring tank 21 through a second discharge hole 20, a second stirring screw 22, a third discharge port 23 is formed in the bottom of the powder stirring tank 21, the third discharge port 23 is connected with a storage tank 24, and the solid-liquid stirring tank 3 and the powder stirring tank 21 are respectively placed under a gamma-ray radiation source for stirring; the specific operation is carried out according to the following steps:
modification of potassium feldspar:
weighing 10kg of potassium feldspar with the grain size of 800 meshes, treating the potassium feldspar for 12 hours by using 20kg of dilute hydrochloric acid solution with the mass concentration of 0.01%, and roasting the potassium feldspar for 5 hours in an air atmosphere at the temperature of 300 ℃;
modification of vermiculite:
weighing 10kg of vermiculite with the particle size of 500 meshes, treating the vermiculite with 20kg of 1% sodium chloride solution for 12 hours, and roasting the vermiculite for 5 hours in an air atmosphere at the temperature of 300 ℃;
preparing a polyethylene glycol aqueous solution:
weighing 1000g of polyethylene glycol-400, dissolving in 10000g of water, mixing to obtain a polyethylene glycol aqueous solution, weighing 5kg of the polyethylene glycol aqueous solution, and adding into a solution preparation tank 5;
respectively weighing 1kg of modified potassium feldspar, 1kg of modified vermiculite, 0.2kg of high index surface titanium dioxide, 0.1kg of sodium titanate, 0.01kg of boron nitride and 0.05kg of carbon nitride, adding the weighed materials into a dry powder mixing tank 1, and stirring for 2 hours to obtain mixed powder;
transferring the obtained mixed powder into a solid-liquid stirring tank 3 through a first powder conveying pipe 2, and uniformly spraying 5kg of polyethylene glycol aqueous solution in a solution preparation tank 5 into the solid-liquid stirring tank 3 through a solution conveying pipe 6, a solution spraying pipe 7 and a solution nozzle 8 to obtain suspension;
starting the first stirring screw 4, stirring the mixed suspension for 1 hour, then placing the solid-liquid stirring tank 3 under gamma rays 9 for irradiation for 5 hours, wherein the radiation dose of the gamma rays is 500rad/s, the first stirring screw 4 in the solid-liquid stirring tank 3 is always opened while the irradiation is carried out, and the suspension is always in a high-speed stirring state;
after the radiation is finished, the suspension in the solid-liquid stirring tank 3 is transferred into a suspension collection tank 11 through a first discharge port 10, a stirrer 12 arranged in the suspension collection tank 11 is always started, and the suspension is always in a high-speed stirring state;
transferring the suspension in the suspension collection tank 11 into a spray dryer 16 through a suspension conveying pipe 15 for spray drying, transferring the spray-dried powder into a powder collector 17, then transferring the powder into a continuous carbonization furnace 19 through a second powder conveying pipe 18, roasting at 400 ℃ for 1 hour, transferring the roasted powder into a powder stirring tank 21 through a second discharge port 20, placing the powder stirring tank 21 under gamma rays 9 for irradiation for 1 hour, wherein the radiation dose of the gamma rays is 500rad/s, and simultaneously, a second stirring screw 22 arranged in the powder stirring tank 21 is always opened, and the powder is always in a high-speed stirring state;
after the irradiation is finished, the powder in the powder stirring tank 21 is transferred into a storage tank 24 through a third discharge port 23, and the organic-inorganic composite material rich in crystal defect structures and with the particle size distribution of 60-200 meshes is obtained.
Example 2
The method relates to a device according to the embodiment 1, and the specific operation is carried out according to the following steps:
modification of potassium feldspar:
weighing 10kg of potassium feldspar with the grain size of 800 meshes, treating the potassium feldspar for 12 hours by using 20kg of dilute hydrochloric acid solution with the mass concentration of 0.01%, and roasting the potassium feldspar for 5 hours in an air atmosphere at the temperature of 400 ℃;
modification of vermiculite:
weighing 10kg of vermiculite with the particle size of 500 meshes, treating the vermiculite with 20kg of 1% sodium chloride solution for 12 hours, and roasting the vermiculite for 5 hours in an air atmosphere at the temperature of 400 ℃;
preparing a polyethylene glycol aqueous solution:
weighing 1000g of polyethylene glycol-600, dissolving in 10000g of water to obtain a polyethylene glycol aqueous solution, weighing 5kg of the polyethylene glycol aqueous solution, and adding into a solution preparation tank 5;
respectively weighing 0.95kg of modified potassium feldspar, 0.95kg of modified vermiculite, 0.2kg of high index surface titanium dioxide, 0.15kg of sodium titanate, 0.01kg of boron nitride and 0.05kg of carbon nitride, adding the materials into a powder mixer, and stirring for 2 hours to obtain mixed powder;
transferring the obtained mixed powder into a solid-liquid stirring tank 3 through a first powder conveying pipe 2, and uniformly spraying 5kg of polyethylene glycol aqueous solution in a solution preparation tank 5 into the solid-liquid stirring tank 3 through a solution conveying pipe 6, a solution spraying pipe 7 and a solution nozzle 8 to obtain suspension;
starting the first stirring screw 4, stirring the suspension for 1 hour, and then placing the solid-liquid stirring tank 3 under gamma ray 9 for irradiation for 1 hour, wherein the radiation dose of the gamma ray is as follows: 0.002rad/s, wherein the first stirring screw 4 in the solid-liquid stirring tank 3 is always opened while radiating, and the suspension is always in a high-speed stirring state;
after the radiation is finished, the suspension in the solid-liquid stirring tank 3 is transferred into a suspension collection tank 11 through a first discharge port 10, a stirrer 12 arranged in the suspension collection tank 11 is always started, and the suspension is always in a high-speed stirring state;
the suspension in the suspension collecting tank 11 is transferred into a spray dryer 16 through a suspension conveying pipe 15 for spray drying, the powder after spray drying is transferred into a powder collector 17, then the powder is transferred into a continuous carbonization furnace 19 through a second powder conveying pipe 18, the powder is roasted at the temperature of 60 ℃ for 1 hour, the roasted powder is transferred into a powder stirring tank 21 through a second discharge port 20, the powder stirring tank 21 is placed under gamma rays 9 for irradiation for 2 hours, and the radiation dose of the gamma rays is as follows: 0.002rad/s, the second stirring screw 22 arranged in the powder stirring tank is always opened while irradiating, and the powder is always in a high-speed stirring state;
after the irradiation is finished, the powder in the powder stirring tank 21 is transferred into a storage tank 24 through a third discharge port 23, and the organic-inorganic composite material rich in crystal defect structures and with the particle size distribution of 60-200 meshes is obtained.
Example 3
The method relates to a device according to the embodiment 1, and the specific operation is carried out according to the following steps:
modification of potassium feldspar:
weighing 10kg of potassium feldspar with the grain size of 800 meshes, treating the potassium feldspar for 12 hours by using 20kg of dilute hydrochloric acid solution with the mass concentration of 0.01%, and roasting the potassium feldspar for 5 hours in an air atmosphere at the temperature of 300 ℃;
modification of vermiculite:
weighing 10kg of vermiculite with the particle size of 500 meshes, treating the vermiculite with 20kg of 1% sodium chloride solution for 12 hours, and roasting the vermiculite for 5 hours in an air atmosphere at the temperature of 300 ℃;
preparing a polyethylene glycol aqueous solution:
weighing 1000g of polyethylene glycol-200, dissolving in 10000g of water to obtain a polyethylene glycol aqueous solution, weighing 5kg of the polyethylene glycol aqueous solution, and adding into a solution preparation tank 5;
respectively weighing 0.8kg of modified potassium feldspar, 0.8kg of modified vermiculite, 0.3kg of high index surface titanium dioxide, 0.3kg of sodium titanate, 0.01kg of boron nitride and 0.05kg of carbon nitride, adding the materials into a powder mixer, and stirring for 2 hours to obtain mixed powder;
transferring the obtained mixed powder into a solid-liquid stirring tank 3 through a first powder conveying pipe 2, and uniformly spraying the polyethylene glycol aqueous solution in a solution preparation tank 5 into the solid-liquid stirring tank 3 through a solution conveying pipe 6, a solution spraying pipe 7 and a solution nozzle 8 to obtain a suspension;
starting the first stirring screw 4, stirring the suspension liquid in the step b for 1 hour, and then placing the solid-liquid stirring tank 3 under gamma rays 9 for irradiation for 3 hours, wherein the radiation dose of the gamma rays is as follows: 1.0rad/s, wherein the first stirring screw 4 in the stirring tank is always opened while radiation is carried out, and the suspension is always in a high-speed stirring state;
after the radiation is finished, the suspension in the solid-liquid stirring tank 3 is transferred into a suspension collection tank 11 through a first discharge port 10, a stirrer 12 arranged in the suspension collection tank 11 is always started, and the suspension is always in a high-speed stirring state;
the suspension in the suspension collecting tank 11 is transferred into a spray dryer 16 through a suspension conveying pipe 15 for spray drying, the powder after spray drying is transferred into a powder collector 17, then the powder is transferred into a continuous carbonization furnace 19 through a second powder conveying pipe 18, the powder is roasted at the temperature of 80 ℃ for 2 hours, the roasted powder is transferred into a powder stirring tank 21 through a second discharge port 20, the powder stirring tank 21 is placed under gamma rays 9 for irradiation for 3 hours, and the radiation dose of the gamma rays is as follows: 1.0rad/s, the second stirring screw 22 arranged in the powder stirring tank is always opened while the powder is irradiated, and the powder is always in a high-speed stirring state;
after the irradiation is finished, the powder material in the powder stirring tank 21 is transferred into a material storage tank 24 through a third discharge port 23, and the organic-inorganic composite material rich in crystal defect structures and with the particle size distribution of 60-200 meshes is obtained.
Example 4
The method relates to a device according to the embodiment 1, and the specific operation is carried out according to the following steps:
modification of potassium feldspar:
weighing 10kg of potassium feldspar with the grain size of 800 meshes, treating the potassium feldspar for 12 hours by using 20kg of dilute hydrochloric acid solution with the mass concentration of 0.01%, and roasting the potassium feldspar for 5 hours in an air atmosphere at the temperature of 300 ℃;
modification of vermiculite:
weighing 10kg of vermiculite with the particle size of 500 meshes, treating the vermiculite with 20kg of 1% sodium chloride solution for 12 hours, and roasting the vermiculite for 5 hours in an air atmosphere at the temperature of 300 ℃;
preparing a polyethylene glycol aqueous solution:
weighing 1000g of polyethylene glycol-800, dissolving in 10000g of water to obtain a polyethylene glycol aqueous solution, weighing 5kg of the polyethylene glycol aqueous solution, and adding into a solution preparation tank 5;
respectively weighing 0.7kg of modified potassium feldspar, 0.7kg of modified vermiculite, 0.4kg of high index surface titanium dioxide, 0.3kg of sodium titanate, 0.02kg of boron nitride and 0.08kg of carbon nitride, adding the materials into a powder mixer, and stirring for 2 hours to obtain mixed powder;
transferring the obtained mixed powder into a solid-liquid stirring tank 3 through a first powder conveying pipe 2, and uniformly spraying the polyethylene glycol aqueous solution in a solution preparation tank 5 into the solid-liquid stirring tank 3 through a solution conveying pipe 6, a solution spraying pipe 7 and a solution nozzle 8 to obtain a suspension;
starting the first stirring screw 4, stirring the suspension liquid in the step b for 1 hour, and then placing the solid-liquid stirring tank 3 under gamma rays 9 for irradiation for 4 hours, wherein the radiation dose of the gamma rays is as follows: 10rad/s, wherein the first stirring screw 4 arranged in the solid-liquid stirring tank 3 is always opened while radiation is carried out, and the suspension is always in a high-speed stirring state;
after the radiation is finished, the suspension in the solid-liquid stirring tank 3 is transferred into a suspension collection tank 11 through a first discharge port 10, a stirrer 12 arranged in the suspension collection tank 11 is always started, and the suspension is always in a high-speed stirring state;
the suspension in the suspension collecting tank 11 is transferred into a spray dryer 16 through a suspension conveying pipe 15 for spray drying, the powder after spray drying is transferred into a powder collector 17, then the powder is transferred into a continuous carbonization furnace 19 through a second powder conveying pipe 18, the powder is roasted for 3 hours at the temperature of 100 ℃, the roasted powder is transferred into a powder stirring tank 21 through a second discharge port 20, the powder stirring tank 21 is placed under gamma rays 9 for irradiation for 4 hours, and the radiation dose of the gamma rays is as follows: 100rad/s, wherein the second stirring screw 22 arranged in the powder stirring tank 21 is always opened while the powder is irradiated, and the powder is always in a high-speed stirring state;
after the irradiation is finished, the powder in the powder stirring tank 21 is transferred into a storage tank 24 through a third discharge port 23, and the organic-inorganic composite material rich in crystal defect structures and with the particle size distribution of 60-200 meshes is obtained.
Example 5
The method relates to a device according to the embodiment 1, and the specific operation is carried out according to the following steps:
modification of potassium feldspar:
weighing 10kg of potassium feldspar with the grain size of 800 meshes, treating the potassium feldspar for 12 hours by using 20kg of dilute hydrochloric acid solution with the mass concentration of 0.01%, and roasting the potassium feldspar for 5 hours in an air atmosphere at the temperature of 300 ℃;
modification of vermiculite:
weighing 10kg of vermiculite with the particle size of 500 meshes, treating the vermiculite with 20kg of 1% sodium chloride solution for 12 hours, and roasting the vermiculite for 5 hours in an air atmosphere at the temperature of 300 ℃;
preparing a polyethylene glycol aqueous solution:
weighing 1000g of polyethylene glycol-1000, dissolving in 10000g of water to obtain a polyethylene glycol aqueous solution, weighing 5kg of the polyethylene glycol aqueous solution, and adding into a solution preparation tank 5;
respectively weighing 0.6kg of modified potassium feldspar, 0.6kg of modified vermiculite, 0.6kg of high index surface titanium dioxide, 0.2kg of sodium titanate, 0.01kg of boron nitride and 0.05kg of carbon nitride, adding the materials into a powder mixer, and stirring for 2 hours to obtain mixed powder;
transferring the obtained mixed powder into a solid-liquid stirring tank 3 through a first powder conveying pipe 2, and uniformly spraying the polyethylene glycol aqueous solution in a solution preparation tank 5 into the solid-liquid stirring tank 3 through a solution conveying pipe 6, a solution spraying pipe 7 and a solution nozzle 8 to obtain a suspension;
starting the first stirring screw 4, stirring the suspension obtained in the step b for 1 hour, then placing the solid-liquid stirring tank 3 under gamma rays 9 for irradiation for 4 hours, wherein the radiation dose of the gamma rays is 500rad/s, and the first stirring screw 4 arranged in the solid-liquid stirring tank 3 is always started while the radiation is carried out, so that the suspension is always in a high-speed stirring state;
after the radiation is finished, the suspension in the solid-liquid stirring tank 3 is transferred into a suspension collection tank 11 through a first discharge port 10, a stirrer 12 arranged in the suspension collection tank 11 is always started, and the suspension is always in a high-speed stirring state;
the suspension in the suspension collecting tank 11 is transferred into a spray dryer 16 through a suspension conveying pipe 15 for spray drying, the powder after spray drying is transferred into a powder collector 17, then the powder is transferred into a continuous carbonization furnace 19 through a second powder conveying pipe 18, the powder is roasted for 4 hours at the temperature of 200 ℃, the roasted powder is transferred into a powder stirring tank 21 through a second discharge port 20, the powder stirring tank 21 is placed under gamma rays 9 for irradiation for 4 hours, and the radiation dose of the gamma rays is as follows: 500rad/s, the second stirring screw 22 arranged in the powder stirring tank 21 is always opened while irradiating, and the powder is always in a high-speed stirring state;
after the irradiation is finished, the powder in the powder stirring tank 21 is transferred into a storage tank 24 through a third discharge port 23, and the organic-inorganic composite material rich in crystal defect structures and with the particle size distribution of 60-200 meshes is obtained.
Example 6
The method relates to a device according to the embodiment 1, and the specific operation is carried out according to the following steps:
modification of potassium feldspar:
weighing 10kg of potassium feldspar with the grain size of 800 meshes, treating the potassium feldspar for 12 hours by using 20kg of dilute hydrochloric acid solution with the mass concentration of 0.01%, and roasting the potassium feldspar for 5 hours in an air atmosphere at the temperature of 300 ℃;
modification of vermiculite:
weighing 10kg of vermiculite with the particle size of 500 meshes, treating the vermiculite with 20kg of 1% sodium chloride solution for 12 hours, and roasting the vermiculite for 5 hours in an air atmosphere at the temperature of 300 ℃;
preparing a polyethylene glycol aqueous solution:
weighing 1000g of polyethylene glycol-2000, dissolving in 10000g of water to obtain a polyethylene glycol aqueous solution, weighing 5kg of the polyethylene glycol aqueous solution, and adding into a solution preparation tank 5;
respectively weighing 0.5kg of modified potassium feldspar, 0.5kg of modified vermiculite, 0.7kg of high index surface titanium dioxide, 0.2kg of sodium titanate, 0.02kg of boron nitride and 0.1kg of carbon nitride, adding the materials into a powder mixer, and stirring for 2 hours to obtain mixed powder;
transferring the obtained mixed powder into a solid-liquid stirring tank 3 through a first powder conveying pipe 2, and uniformly spraying the polyethylene glycol aqueous solution in a solution preparation tank 5 into the solid-liquid stirring tank 3 through a solution conveying pipe 6, a solution spraying pipe 7 and a solution nozzle 8 to obtain a suspension;
starting the first stirring screw 4, stirring the suspension obtained in the step b for 1 hour, then placing the solid-liquid stirring tank 3 under gamma rays 9 for irradiation for 5 hours, wherein the radiation dose of the gamma rays is 1000rad/s, and the first stirring screw 4 arranged in the solid-liquid stirring tank 3 is always started while the radiation is carried out, so that the suspension is always in a high-speed stirring state;
after the radiation is finished, the suspension in the solid-liquid stirring tank 3 is transferred into a suspension collection tank 11 through a first discharge port 10, a stirrer 12 arranged in the suspension collection tank 11 is always started, and the suspension is always in a high-speed stirring state;
the suspension in the suspension collecting tank 11 is transferred into a spray dryer 16 through a suspension conveying pipe 15 for spray drying, the powder after spray drying is transferred into a powder collector 17, then is transferred into a continuous carbonization furnace 19 through a second powder conveying pipe 18 for roasting at 300 ℃ for 5 hours, the roasted powder is transferred into a powder stirring tank 21 through a second discharge port 20, the powder stirring tank 21 is placed under gamma rays 9 for irradiation for 5 hours, and the radiation dose of the gamma rays is as follows: 1000rad/s, the second stirring screw 22 arranged in the powder stirring tank 21 is always opened while irradiating, and the powder is always in a high-speed stirring state;
after the irradiation is finished, the powder in the powder stirring tank 21 is transferred into a storage tank 24 through a third discharge port 23, and the organic-inorganic composite material rich in crystal defect structures and with the particle size distribution of 60-200 meshes is obtained.
Example 7
The dynamic adsorption performance of any one of the organic-inorganic composite materials of examples 1 to 6 on nickel, cobalt, lead, cadmium, mercury, chromium and arsenic was studied by using a test apparatus:
weighing 100g of organic-inorganic composite material, putting the organic-inorganic composite material into a filter bottle, enabling a mixed solution of nickel, cobalt, lead, cadmium, mercury, chromium and arsenic ions of various heavy metal ions to enter the filter bottle filled with the organic-inorganic composite material from a water inlet, then dynamically flowing and completing adsorption, discharging the adsorbed mixed solution from a water outlet, measuring the content of nickel, cobalt, lead, cadmium, mercury, chromium and arsenic in water flowing out of the water outlet, respectively inspecting the influence of the concentration of the nickel, cobalt, lead, cadmium, mercury, chromium and arsenic on the dynamic adsorption performance, respectively setting the concentration of the nickel, cobalt, lead, cadmium, mercury, chromium and arsenic to be 10ppb, 20ppb, 40ppb, 60ppb, 80ppb, 100ppb, 150ppb and 200ppb, and inspecting the influence of the initial concentration on the adsorption performance, wherein the table 1 shows.
Example 8
The dynamic adsorption performance of any one of the organic-inorganic composite materials of examples 1 to 6 on nickel, cobalt, lead, cadmium, mercury, chromium and arsenic was studied by using a test apparatus:
weighing 100g of organic-inorganic composite material, putting the organic-inorganic composite material into a filter bottle, enabling mixed liquor of nickel, cobalt, lead, cadmium, mercury, chromium and arsenic ions of various heavy metal ions to enter the filter bottle filled with the organic-inorganic composite material from a water inlet, then dynamically flowing and completing adsorption, discharging the adsorbed mixed liquor from a water outlet, measuring the content of nickel, cobalt, lead, cadmium, mercury, chromium and arsenic in water flowing out of the water outlet, respectively inspecting the influence of the concentration of the nickel, cobalt, lead, cadmium, mercury, chromium and arsenic on the dynamic adsorption performance, respectively setting the concentration of the nickel, cobalt, lead, cadmium, mercury, chromium and arsenic to be 250ppb, 300ppb, 350ppb, 400ppb, 450ppb and 500ppb, and inspecting the influence of initial concentration on the adsorption performance, wherein the table 1:
table 1 shows the removal rates of the material in example 1 of the present invention for nickel, cobalt, lead, cadmium, mercury, chromium and arsenic at different concentrations in the mixed aqueous solution
Figure BDA0002760563840000091
Figure BDA0002760563840000092
Figure BDA0002760563840000093
Figure BDA0002760563840000094
Figure BDA0002760563840000095
Figure BDA0002760563840000096
Figure BDA0002760563840000101
Table 2 shows the removal rates of the material of example 10 (comparative example 1) of the present invention for nickel, cobalt, lead, cadmium, mercury, chromium and arsenic at different concentrations in the mixed aqueous solution
Figure BDA0002760563840000102
Figure BDA0002760563840000103
Figure BDA0002760563840000104
Figure BDA0002760563840000105
Figure BDA0002760563840000106
Figure BDA0002760563840000107
Table 3 shows the removal rates of the material of example 11 (comparative example 2) of the present invention for nickel, cobalt, lead, cadmium, mercury, chromium and arsenic at different concentrations in the mixed aqueous solution
Figure BDA0002760563840000111
Figure BDA0002760563840000112
Figure BDA0002760563840000113
Figure BDA0002760563840000114
Figure BDA0002760563840000115
Figure BDA0002760563840000116
Example 9
The dynamic adsorption performance of any one of the organic-inorganic composite materials of examples 1 to 6 on nickel, cobalt, lead, cadmium, mercury, chromium and arsenic was studied by using a test apparatus:
weighing 100g of organic-inorganic composite material, filling the organic-inorganic composite material into a filter bottle, enabling a mixed solution of nickel, cobalt, lead, cadmium, mercury, chromium and arsenic ions of various heavy metal ions to enter the filter bottle filled with the organic-inorganic composite material from a water inlet, then dynamically flowing and completing adsorption, discharging the adsorbed mixed solution from a water outlet, measuring the content of nickel, cobalt, lead, cadmium, mercury, chromium and arsenic in water flowing out of the water outlet, respectively inspecting the influence of the concentration of the nickel, the cobalt, the lead, the cadmium, the mercury, the chromium and the arsenic on the dynamic adsorption performance, respectively setting the concentration of the nickel, the cobalt, the lead, the cadmium, the mercury, the chromium and the arsenic to be 10ppb, 20ppb, 40ppb, 60ppb, 80ppb, 100ppb, 150ppb and 200ppb, inspecting the influence of water flow speed on the adsorption performance, respectively setting the water flow speed to be 0.5L/min, 1L/min, 1.5L/min, 2L/min, 2.5L/min, 2, 3L/min, 3.5L/min, 4L/min, 4.5L/min, 5L/min.
Example 10 (comparison with example 1)
The device and the operation steps are the same as those of the embodiment 1, and the difference from the embodiment 1 is that the whole production process does not receive gamma ray irradiation;
modification of potassium feldspar:
weighing 10kg of potassium feldspar with the grain size of 800 meshes, treating the potassium feldspar for 12 hours by using 20kg of dilute hydrochloric acid solution with the mass concentration of 0.01%, and roasting the potassium feldspar for 5 hours in an air atmosphere at the temperature of 300 ℃;
modification of vermiculite:
weighing 10kg of vermiculite with the particle size of 500 meshes, treating the vermiculite with 20kg of 1% sodium chloride solution for 12 hours, and roasting the vermiculite for 5 hours in an air atmosphere at the temperature of 300 ℃;
preparing a polyethylene glycol aqueous solution:
weighing 1000g of polyethylene glycol-400, dissolving in 10000g of water to obtain a polyethylene glycol aqueous solution, weighing 5kg of the polyethylene glycol aqueous solution, and adding into a solution preparation tank 5;
respectively weighing 1kg of modified potassium feldspar, 1kg of modified vermiculite, 0.2kg of high index surface titanium dioxide, 0.1kg of sodium titanate, 0.01kg of boron nitride and 0.05kg of carbon nitride, adding the materials into a powder mixer, and stirring for 2 hours to obtain mixed powder;
transferring the obtained mixed powder into a solid-liquid stirring tank 3 through a first powder conveying pipe 2, and uniformly spraying the polyethylene glycol aqueous solution in a solution preparation tank 5 into the solid-liquid stirring tank 3 through a solution conveying pipe 6, a solution spraying pipe 7 and a solution nozzle 8 to obtain turbid liquid;
and (b) starting the first stirring screw 4, stirring the suspension obtained in the step (b) for 1 hour, transferring the suspension into a spray dryer 16 through a suspension conveying pipe 15 for spray drying, transferring the spray-dried powder into a powder collector 17, transferring into a continuous carbonization furnace 19 through a second powder conveying pipe 18, and roasting at the temperature of 400 ℃ for 1 hour to obtain the organic-inorganic composite material rich in the crystal form defect structure and with the particle size distribution of 60-200 meshes.
The removal rate of the material in example 10 of the present invention (comparative example 1) was shown in table 2 for the removal of nickel, cobalt, lead, cadmium, mercury, chromium, and arsenic at different concentrations in the mixed aqueous solution.
Example 11 (comparison with example 1)
The production device and the operation steps are the same as those of the embodiment 1, and the difference from the embodiment 1 is that the high-index surface titanium dioxide, the sodium titanate, the boron nitride and the carbon nitride are not added;
modification of potassium feldspar:
weighing 10kg of potassium feldspar with the grain size of 800 meshes, treating the potassium feldspar for 12 hours by using 20kg of dilute hydrochloric acid solution with the mass concentration of 0.01%, and roasting the potassium feldspar for 5 hours in an air atmosphere at the temperature of 300 ℃;
modification of vermiculite:
weighing 10kg of vermiculite with the particle size of 500 meshes, treating the vermiculite with 20kg of 1% sodium chloride solution for 12 hours, and roasting the vermiculite for 5 hours in an air atmosphere at the temperature of 300 ℃;
preparing a polyethylene glycol aqueous solution:
weighing 1000g of polyethylene glycol-400, dissolving in 10000g of water to obtain a polyethylene glycol aqueous solution, weighing 5kg of the polyethylene glycol aqueous solution, and adding into a solution preparation tank 5;
respectively weighing 1kg of modified potassium feldspar and 1kg of modified vermiculite, adding into a powder mixer, and stirring for 2 hours to obtain mixed powder;
transferring the obtained mixed powder into a solid-liquid stirring tank 3 through a first powder conveying pipe 2, and uniformly spraying the polyethylene glycol aqueous solution in a solution preparation tank 5 into the solid-liquid stirring tank 3 through a solution conveying pipe 6, a solution spraying pipe 7 and a solution nozzle 8 to obtain a suspension;
starting the first stirring screw 4, stirring the suspension obtained in the step b for 1 hour, then placing the solid-liquid stirring tank 3 under gamma rays 9 for irradiation for 5 hours, wherein the radiation dose of the gamma rays is 500rad/s, the first stirring screw 4 in the stirring tank is always opened while the irradiation is carried out, and the suspension is always in a high-speed stirring state;
after the radiation is finished, the suspension in the solid-liquid stirring tank 3 is transferred into a suspension collection tank 11 through a first discharge port 10, a stirrer 12 arranged in the suspension collection tank 11 is always started, and the suspension is always in a high-speed stirring state;
transferring the suspension in the suspension collection tank 11 into a spray dryer 16 through a suspension conveying pipe 15 for spray drying, transferring the spray-dried powder into a powder collector 17, transferring the powder into a continuous carbonization furnace 19 through a second powder conveying pipe 18, roasting at 400 ℃ for 1 hour, transferring the roasted powder into a powder stirring tank 21 through a second discharge port 20, and placing the powder stirring tank 21 under gamma rays 9 for irradiation for 5 hours, wherein the radiation dose of the gamma rays is as follows: 500rad/s, the second stirring screw 22 in the powder stirring tank is always opened while the powder is irradiated, and the powder is always in a high-speed stirring state;
after the irradiation is finished, the powder in the powder stirring tank 21 is transferred into a storage tank 24 through a third discharge port 23, and the organic-inorganic composite material rich in crystal defect structures and with the particle size distribution of 60-200 meshes is obtained.
The removal rates of the material in inventive example 11 (comparative example 2) for different concentrations of nickel, cobalt, lead, cadmium, mercury, chromium and arsenic in the mixed aqueous solution are shown in table 3.
The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.

Claims (2)

1. The method is characterized in that the device is composed of a dry powder mixing tank (1), a first powder conveying pipe (2), a solid-liquid stirring tank (3), a first stirring screw (4), a solution preparation tank (5), a solution conveying pipe (6), a solution spraying pipe (7), a solution nozzle (8), a gamma ray radiation source (9), a first discharge hole (10), a suspension collecting tank (11), a stirrer (12), a support (13), a moving wheel (14), a suspension conveying pipe (15), a spray dryer (16), a powder collector (17), a second powder conveying pipe (18), a continuous carbonization furnace (19), a second discharge hole (20), a powder stirring tank (21), a second stirring screw (22), a third discharge hole (23), The dry powder mixing device comprises a storage tank (24), a dry powder mixing tank (1) is connected with a solid-liquid stirring tank (3) through a first powder conveying pipe (2), a first stirring screw (4) is arranged in the solid-liquid stirring tank (3), a solution preparation tank (5) is arranged at the top end of the solid-liquid stirring tank (3), the solution preparation tank (5) is connected with a solution spraying pipe (7) through a solution conveying pipe (6), a plurality of solution nozzles (8) which are arranged evenly are arranged on the solution spraying pipe (7), a first discharge port (10) is arranged at the bottom of the solid-liquid stirring tank (3), the first discharge port (10) is connected with a suspension collecting tank (11), a stirrer (12) is arranged in the suspension collecting tank (11), suspension is fixed at two ends of the bottom of the solid-liquid stirring tank (3) by a support (13) with movable wheels (14), and the bottom of the suspension collecting tank (11) is connected with a spray dryer (16) through, a powder collector (17) is arranged at the bottom of the spray dryer (16), the powder collector (17) is connected with one end of a continuous carbonization furnace (19) through a second powder conveying pipe (18), the other end of the continuous carbonization furnace (19) is connected with a powder stirring tank (21) through a second discharge hole (20), a second stirring screw (22) is arranged in the powder stirring tank (21), a third discharge hole (23) is arranged at the bottom of the powder stirring tank (21), the third discharge hole (23) is connected with a storage tank (24), and the solid-liquid stirring tank (3) and the powder stirring tank (21) are respectively arranged under a gamma-ray radiation source for stirring; the method takes modified potash feldspar, modified vermiculite, high index surface titanium dioxide, sodium titanate, boron nitride, carbon nitride, polyethylene glycol and water as raw materials, adopts gamma-ray radiation, spray drying, roasting in inert atmosphere and then gamma-ray radiation, and concretely comprises the following steps:
a. respectively mixing modified potash feldspar, modified vermiculite, high index surface titanium dioxide, sodium titanate, boron nitride and carbon nitride in a mass ratio of 0.01-1:0.01-1:0.01-1:0.01-1, and fully stirring to obtain mixed powder;
b. dissolving polyethylene glycol in water according to the mass ratio of 0.01-1:1-10 to obtain a polyethylene glycol aqueous solution, putting the polyethylene glycol aqueous solution into a solution preparation tank (5), transferring the mixed powder obtained in the step a into a solid-liquid stirring tank (3) through a first powder conveying pipe (2), and uniformly spraying the polyethylene glycol aqueous solution in the solution preparation tank (5) into the solid-liquid stirring tank (3) through a solution conveying pipe (6), a solution spraying pipe (7) and a solution nozzle (8) to obtain a suspension, wherein the polyethylene glycol is PEG-200, PEG-400, PEG-600, PEG-800, PEG-1000 or PEG-200; 0
c. Starting a first stirring screw (4), stirring the suspension liquid in the step b for 1 hour, and then placing a solid-liquid stirring tank (3) under gamma rays (9) for irradiation for 1-5 hours, wherein the radiation dose of the gamma rays is as follows: 0.002 rad/s-1000 rad/s, wherein a first stirring screw (4) in the solid-liquid stirring tank (3) is always opened while radiation is carried out, the suspension is always in a high-speed stirring state, after the radiation is finished, the suspension in the solid-liquid stirring tank (3) is transferred into a suspension collecting tank (11) through a first discharge port (10), a stirrer (12) arranged in the suspension collecting tank (11) is always opened, and the suspension is always in a high-speed stirring state;
d. the suspension in the suspension collecting tank (11) is transferred into a spray dryer (16) through a suspension conveying pipe (15) for spray drying, the powder after spray drying is transferred into a powder collector (17), then the powder is transferred into a continuous carbonization furnace (19) through a second powder conveying pipe (18), the powder is roasted for 1 to 5 hours at the temperature of between 60 and 300 ℃, the roasted powder is transferred into a powder stirring tank (21) through a second discharge hole (20), the powder stirring tank (21) is placed under gamma rays (9) for irradiation for 1 to 5 hours, and the radiation dose of the gamma rays is as follows: 0.002 rad/s-1000 rad/s, the second stirring screw (22) in the powder stirring tank (21) is always opened while the powder is irradiated, and the powder is always in a high-speed stirring state;
e. after the irradiation is finished, the powder in the powder stirring tank (21) is transferred into a storage tank (24) through a third discharge hole (23), and the organic-inorganic composite material rich in crystal defect structures and with the grain size distribution of 60-200 meshes is obtained.
2. Use of the organic-inorganic composite material obtained by the method of claim 1 for preparing a composite material for simultaneously removing nickel, cobalt, lead, cadmium, mercury, chromium and arsenic ions, which are heavy metal ions.
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115715990A (en) * 2022-11-15 2023-02-28 塔里木大学 g-C 3 N 4 vermiculite/TiO 2 Preparation method and application of ternary composite material

Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103570015A (en) * 2013-09-26 2014-02-12 蚌埠华纺滤材有限公司 Fingered citron slag activated carbon and preparation method thereof
CN204911527U (en) * 2015-06-09 2015-12-30 浙江工业大学 Energy -saving mud of sled dress formula base adsorbent preparation facilities
CN105381790A (en) * 2015-11-04 2016-03-09 苏州书瑞环保科技有限公司 Water treatment chromium adsorbing material and preparation method thereof
CN107213881A (en) * 2017-06-28 2017-09-29 中国科学院新疆理化技术研究所 A kind of Preparation method and use of activated carbon base Inorganic whisker section bar material
CN108295830A (en) * 2018-01-18 2018-07-20 中国建筑材料科学研究总院有限公司 The TiO of 001,101 crystal faces of exposure2/ sepiolite plural gel and preparation method thereof
CN108503045A (en) * 2018-04-12 2018-09-07 昆明铜龙科技开发有限公司 Composite highly effective water purification agent and preparation method thereof
CN109250693A (en) * 2018-10-10 2019-01-22 深圳烯材科技有限公司 A kind of method that mechanical force intercalation stripping prepares inorganic two-dimension nano materials
CN109718831A (en) * 2017-10-31 2019-05-07 中国石油化工股份有限公司 Prepare the method and Cracking catalyst of Cracking catalyst
CN110721658A (en) * 2019-10-15 2020-01-24 江苏索普（集团）有限公司 Preparation method and application of hexagonal boron nitride-graphite phase carbon nitride intercalation composite material
CN111397326A (en) * 2020-04-02 2020-07-10 蔡国梁 Method for preparing sewage treatment adsorbent granular activated carbon by molding
CN111841500A (en) * 2020-08-26 2020-10-30 华能国际电力股份有限公司 Method and system for synthesizing VOCs adsorbent by using fly ash and waste oil

Patent Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103570015A (en) * 2013-09-26 2014-02-12 蚌埠华纺滤材有限公司 Fingered citron slag activated carbon and preparation method thereof
CN204911527U (en) * 2015-06-09 2015-12-30 浙江工业大学 Energy -saving mud of sled dress formula base adsorbent preparation facilities
CN105381790A (en) * 2015-11-04 2016-03-09 苏州书瑞环保科技有限公司 Water treatment chromium adsorbing material and preparation method thereof
CN107213881A (en) * 2017-06-28 2017-09-29 中国科学院新疆理化技术研究所 A kind of Preparation method and use of activated carbon base Inorganic whisker section bar material
CN109718831A (en) * 2017-10-31 2019-05-07 中国石油化工股份有限公司 Prepare the method and Cracking catalyst of Cracking catalyst
CN108295830A (en) * 2018-01-18 2018-07-20 中国建筑材料科学研究总院有限公司 The TiO of 001,101 crystal faces of exposure2/ sepiolite plural gel and preparation method thereof
CN108503045A (en) * 2018-04-12 2018-09-07 昆明铜龙科技开发有限公司 Composite highly effective water purification agent and preparation method thereof
CN109250693A (en) * 2018-10-10 2019-01-22 深圳烯材科技有限公司 A kind of method that mechanical force intercalation stripping prepares inorganic two-dimension nano materials
CN110721658A (en) * 2019-10-15 2020-01-24 江苏索普（集团）有限公司 Preparation method and application of hexagonal boron nitride-graphite phase carbon nitride intercalation composite material
CN111397326A (en) * 2020-04-02 2020-07-10 蔡国梁 Method for preparing sewage treatment adsorbent granular activated carbon by molding
CN111841500A (en) * 2020-08-26 2020-10-30 华能国际电力股份有限公司 Method and system for synthesizing VOCs adsorbent by using fly ash and waste oil

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
MARYAM (ROZA) YAZDANI ET AL.: "Synthesis, characterization and exploitation of nano-TiO2/feldspar-embedded chitosan beads towards UV-assisted adsorptive abatement of aqueous arsenic (As)", 《CHEMICAL ENGINEERING JOURNAL》 *
张开诚主编: "《化学实验教程》", 28 February 2014, 华中科技大学出版社 *
聂晓等: "高指数晶面二氧化钛对砷、锑的共吸附去除", 《环境化学》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115715990A (en) * 2022-11-15 2023-02-28 塔里木大学 g-C 3 N 4 vermiculite/TiO 2 Preparation method and application of ternary composite material
CN115715990B (en) * 2022-11-15 2023-12-22 塔里木大学 g-C 3 N 4 vermiculite/TiO 2 Preparation method and application of ternary composite material

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