CN111659341A - Phosphonium salt modified high-temple bentonite and preparation method and application thereof - Google Patents
Phosphonium salt modified high-temple bentonite and preparation method and application thereof Download PDFInfo
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/00—Treatment of water, waste water, or sewage
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- G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
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- G21F9/12—Processing by absorption; by adsorption; by ion-exchange
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
The invention discloses a quaternary phosphonium salt modified high-temple bentonite and a preparation method and application thereof, wherein the quaternary phosphonium salt surfactant solution and the high-temple bentonite powder are fully mixed and reacted by utilizing the characteristic that inorganic cations and organic cations of the high-temple bentonite are subjected to ion exchange, and then the quaternary phosphonium salt modified high-temple bentonite powder is prepared by the processes of drying, ultrapure water washing, grinding, sieving and the like, wherein the elements comprise, by mass, 40-50% of oxygen, 25-35% of silicon, 7-8% of aluminum, 1-3% of phosphorus, 8-15% of carbon, 0.1-0.2% of calcium, 0.05-0.2% of sodium, 1.5-1.7% of magnesium, 0.2-0.3% of potassium, 0.6-0.8% of iron, 0.04-0.05% of titanium, 0.02-0.03% of manganese and 0.01-0.01% of chlorine. The modified bentonite has stronger adsorption capacity to anions in wastewater.
Description
Technical Field
The invention belongs to the field of geological disposal of modified bentonite and high-level waste, and particularly relates to quaternary phosphonium salt modified high-temple bentonite and a preparation method and application thereof.
Background
With the continuous development and the large use of nuclear energy, a large amount of radioactive waste is generated, and the radioactive waste can be divided into low-level, medium-level and high-level waste according to the difference of radioactivity size. The high radioactive waste contains radionuclides such as selenium and iodine, the radioactive half-life period of the elements is long, the elements can release heat for a long time, and the elements have high physical toxicity, chemical toxicity and biological toxicity, and based on the prior art, the radioactive waste cannot be further utilized or the harm of the radioactive waste can not be eliminated. Therefore, safe treatment and disposal of high level waste is an important guarantee for the health and sustainable development of nuclear energy.
At present, the internationally accepted and technically feasible solution for disposing high level waste is deep geological disposal, i.e. the high level waste is buried in geological bodies at a depth of 500 to 1000 meters from the surface of the earth, so that the high level waste is permanently isolated from the living environment of human beings. The buffer backfill in high level waste deep geological processing is the last artificial barrier, which is critical to the safety of the high level waste disposal system. At present, bentonite of high temple in Xingmuxing and county is selected as a first-choice candidate material for geological disposal buffer/backfill material of high radioactive waste in China by the characteristics of high expansibility, low water permeability, strong cation exchange capacity, good nuclide (most nuclides) blocking capacity and the like, but because the surface of the bentonite is electronegative, the bentonite has anion exclusion effect, and has key nuclide rejection effect129The adsorption of radioactive anionic nuclides such as I is weak, so that the anionic nuclides are easy to migrate into a biosphere along with groundwater, and harm is caused to the environment and human beings. Therefore, it is necessary to modify the bentonite to prepare a material capable of effectively adsorbing anions so as to enhance the migration retarding capability of the material on the anions.
Disclosure of Invention
In order to overcome the problems in the prior art, the invention aims to provide the quaternary phosphonium salt modified high-temple bentonite capable of effectively adsorbing anions, and the preparation method and the application thereof, so as to overcome the defect of backfill material high-temple bentonite in the aspect of anion retardation.
In order to realize the purpose, the technical scheme of the invention is as follows:
the quaternary phosphonium salt modified high-temple bentonite material is prepared by fully mixing and reacting a quaternary phosphonium salt surfactant solution and high-temple bentonite powder by using the ion exchange between inorganic cation energy and organic cation in the high-temple bentonite.
The invention provides a quaternary phosphonium salt modified high temple bentonite, which comprises, by mass, 40-50% of oxygen, 25-35% of silicon, 7-8% of aluminum, 1-3% of phosphorus, 8-15% of carbon, 0.1-0.2% of calcium, 0.05-0.2% of sodium, 1.5-1.7% of magnesium, 0.2-0.3% of potassium, 0.6-0.8% of iron, 0.04-0.05% of titanium, 0.02-0.03% of manganese and 0.01-0.02% of chlorine.
The second purpose of the invention is to provide a preparation method of the quaternary phosphonium salt modified high temple bentonite, which comprises the following steps:
1) putting the quaternary phosphonium salt surfactant into ultrapure water, stirring while adding until the surfactant is completely dissolved to form a surfactant solution;
2) adding the high-temple bentonite into the surfactant solution obtained in the step 1), stirring while adding until the mixture is uniformly mixed, wherein exchangeable cations among bentonite layers can be replaced by quaternary phosphonium salt cations in the process, so that the quaternary phosphonium salt cations are inserted or covered among the bentonite layers to form modified bentonite combined by covalent bonds, ionic bonds, coupling bonds or Van der Waals forces, and obtaining a modified bentonite suspension;
3) continuously stirring the modified bentonite suspension obtained in the step 2) for a preset time, then carrying out solid-liquid separation in a suction filtration mode, and removing filtrate to obtain a solid;
4) continuously washing the solid obtained in the step 3) with ultrapure water until the redundant quaternary phosphonium salt surfactant is completely washed away;
5) putting the solid washed by the ultrapure water in the step 4) into an oven for drying to obtain a quaternary phosphonium salt modified high-temple bentonite solid;
6) and grinding the quaternary phosphonium salt modified high-temple bentonite solid into powder, and sieving with a 200-mesh sieve to obtain the quaternary phosphonium salt modified high-temple bentonite.
The dosage of the quaternary phosphonium salt surfactant and the bentonite in the step 1) and the step 2) is determined according to the cation exchange capacity, namely the dosage of the quaternary phosphonium salt surfactant: 3.46 mmol-13.84 mmol of bentonite: 10 g.
In the preparation method of the quaternary phosphonium salt modified temple bentonite, the quaternary phosphonium salt surfactant in the step 1) is trihexyltetradecylphosphonium chloride, tetrabutylphosphonium chloride or butyltriphenylphosphonium chloride.
In the preparation method of the quaternary phosphonium salt modified high temple bentonite, in the step 2), the high temple bentonite is calcium-based high temple bentonite, the cation exchange capacity is 69.2mmol/100g, and the high temple bentonite is ground and sieved by a 200-mesh sieve.
In the preparation method of the quaternary phosphonium salt modified high temple bentonite, the stirring in the step 1) and the step 2) is carried out on a constant-temperature magnetic stirrer, the stirring temperature is 25-75 ℃, and the stirring speed is 100-900 r/min; the continuous stirring in the step 3) is carried out for a preset time of 24 h.
In the preparation method of the quaternary phosphonium salt modified homo temple bentonite, whether the redundant quaternary phosphonium salt surfactant is washed off in the step 4) is detected by 0.1mol/L silver nitrate solution, 4-6 drops of silver nitrate solution are added into the filtrate after the ultra-pure water washing, and if no white precipitate is generated, the situation that the redundant quaternary phosphonium salt surfactant is washed off is shown.
In the preparation method of the quaternary phosphonium salt modified high temple bentonite, the drying temperature in the step 5) is 60 ℃.
In the preparation method of the quaternary phosphonium salt modified homo temple bentonite, the sieving in the step 6) is 200-mesh sieving.
The application of quaternary phosphonium salt modified high-temple bentonite material, the modified material is used as adsorbent for removing iodine ions in waste water.
In the application, the dosage of the adsorbent in the wastewater is 1-10g/L, the initial concentration of iodide ions is 0.85-4.23mg/L, the oscillation time is 2-24h, and the temperature is 25-65 ℃.
The invention has the beneficial effects that:
1) the high-temple bentonite used in the invention has higher montmorillonite content, larger cation exchange capacity and specific surface area, and good low permeability, high expansibility and good heat conductivity, and is a preferred candidate material for a buffer/backfill material of a high-level radioactive waste geological repository in China.
2) The raw materials used in the invention have rich sources and low cost, the preparation process of the composite material is simple and easy to control, and the product can be used only by crushing without operations such as purification and the like, so the preparation cost is low.
3) Compared with the hydrophilic and oleophobic properties of the high temple bentonite, due to the introduction of the organic component quaternary phosphonium salt surfactant, the quaternary phosphonium salt modified high temple bentonite has the advantages of hydrophobicity and oleophilicity and lower permeability; and compared with the similar quaternary ammonium salt surfactant, the quaternary phosphonium salt surfactant has higher thermal stability, so that the thermal stability of the quaternary phosphonium salt modified bentonite is better than that of the similar quaternary ammonium salt modified bentonite.
4) As quaternary phosphonium salt cations enter the interlayer domain of the bentonite, the surface property of the bentonite is changed, and electrostatic interaction exists between the quaternary phosphonium salt cations and anions, so that the quaternary phosphonium salt modified Hovenia dulcis bentonita is beneficial to adsorbing the anions, so that the quaternary phosphonium salt modified Hovenia dulcis bentonita has high removal efficiency of iodide ions in wastewater, the adsorption rate can reach more than 70%, and the migration of the iodide ions can be effectively retarded.
Detailed Description
The present embodiment is based on the technical scheme of the invention, and a detailed implementation manner and a specific operation process are given, but the scope of the present invention is not limited to the following embodiments.
Example 1:
a preparation method of quaternary phosphonium salt modified high temple bentonite comprises the following steps:
1) placing a beaker on a constant-temperature magnetic stirrer at room temperature, adding 1L of ultrapure water into the beaker, adding 3.59g (6.92mmol) of trihexyltetradecylphosphine chloride while stirring, wherein the stirring speed is 300r/min until the surfactant is completely dissolved;
2) weighing 10g of calcium-based Lauraria nobilis bentonite, adding the calcium-based Lauraria nobilis bentonite into the surfactant solution obtained in the step 1) at the temperature of 25 ℃ and the stirring speed of 600r/min, and stirring while adding until the calcium-based Lauraria nobilis bentonite is uniformly mixed to obtain a modified bentonite suspension;
3) continuously stirring the modified bentonite suspension obtained in the step 2) for 24 hours, then carrying out solid-liquid separation in a suction filtration mode, removing filtrate, and keeping solids;
4) putting the solid obtained in the step 3) into a beaker, and adding the solid into the beaker according to the weight ratio of ultrapure water: adding ultrapure water according to the mass ratio of the solids of 20:1, stirring, then carrying out suction filtration, removing filtrate, retaining the solids, repeating the ultrapure water washing operation for 6-9 times, adding 4-6 drops of 0.1mol/L silver nitrate solution into the last filtrate, and if no white precipitate is generated, carrying out the step 5), otherwise, continuing the operation of washing the modified bentonite solids with the ultrapure water;
5) putting the solid obtained after the suction filtration in the step 4) into an oven, and drying the sample at the temperature of 60 ℃ to obtain a quaternary phosphonium salt modified high-temple bentonite solid;
6) grinding the obtained quaternary phosphonium salt modified high-temple bentonite solid into powder, and sieving with a 200-mesh sieve to obtain the quaternary phosphonium salt modified high-temple bentonite (T100-GMZ).
The prepared quaternary phosphonium salt modified high-temple bentonite (T100-GMZ) and the calcium-based high-temple bentonite (Ca-GMZ) are respectively subjected to X-ray diffraction fluorescence spectrum analysis to obtain main element components of the bentonite material, and the main element components are shown in Table 1. Compared with Ca-GMZ, the P content of T100-GMZ is increased from 0.02 to 2.21 percent, and the C content is increased from 0 to 12 percent, which indicates that the modification is successful.
TABLE 1 main element composition (percentage) of bentonite
Example 2:
the quaternary phosphonium salt modified high temple bentonite material prepared in the example 1 is applied to the adsorption treatment of iodide ions, and comprises the following steps: adding an iodide ion solution into the adsorbent suspension, wherein the adsorbent concentration in the mixed solution is 5g/L, and the iodide ion concentration is 0.85 mg/L; placing the mixture into an electric heating constant-temperature water bath oscillation water tank for oscillation for 2 hours at the temperature of 25 ℃; under the conditions that the centrifugal speed is 4000r/min and the centrifugal time is 10min, the solid-liquid separation is realized by using a low-speed centrifugal machine, and then the concentration of the unadsorbed iodide ions in the solution is measured by using an ion chromatograph; the percentage of the adsorbed iodide ions was calculated from the difference in the iodide ion concentration between the solution before and after adsorption, and the adsorption rate of T100-GMZ for iodide ions was 41.16%.
Example 3:
the quaternary phosphonium salt modified high temple bentonite material prepared in the example 1 is applied to the adsorption treatment of iodide ions, and comprises the following steps: adding an iodide ion solution into the adsorbent suspension, wherein the adsorbent concentration in the mixed solution is 5g/L, and the iodide ion concentration is 4.23 mg/L; placing the mixture into an electric heating constant-temperature water bath oscillation water tank for oscillation for 24 hours at the temperature of 25 ℃; under the conditions that the centrifugal speed is 4000r/min and the centrifugal time is 10min, the solid-liquid separation is realized by using a low-speed centrifugal machine, and then the concentration of the unadsorbed iodide ions in the solution is measured by using an ion chromatograph; and calculating the adsorbed percentage according to the concentration difference of the iodide ions in the solution before and after adsorption, wherein the adsorption rate of the T100-GMZ on the iodide ions reaches 76.08%.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is intended to include such modifications and variations. The foregoing examples or embodiments are merely illustrative of the present invention, which may be embodied in other specific forms or in other specific forms without departing from the spirit or essential characteristics thereof. The described embodiments are, therefore, to be considered in all respects as illustrative and not restrictive. The scope of the invention should be indicated by the appended claims, and any changes that are equivalent to the intent and scope of the claims should be construed to be included therein.
Claims (9)
1. The quaternary phosphonium salt modified high temple bentonite is characterized in that the quaternary phosphonium salt modified high temple bentonite contains, by mass, 40-50% of oxygen, 25-35% of silicon, 7-8% of aluminum, 1-3% of phosphorus, 8-15% of carbon, 0.1-0.2% of calcium, 0.05-0.2% of sodium, 1.5-1.7% of magnesium, 0.2-0.3% of potassium, 0.6-0.8% of iron, 0.04-0.05% of titanium, 0.02-0.03% of manganese and 0.01-0.02% of chlorine.
2. The method for preparing the quaternary phosphonium salt modified homo temple bentonite according to claim 1, wherein the method comprises the steps of:
1) putting the quaternary phosphonium salt surfactant into ultrapure water, stirring while adding until the surfactant is completely dissolved to form a surfactant solution;
2) adding the high-temple bentonite into the surfactant solution obtained in the step 1), stirring while adding until the mixture is uniformly mixed, wherein exchangeable cations among bentonite layers can be replaced by quaternary phosphonium salt cations in the process, so that the quaternary phosphonium salt cations are inserted or covered among the bentonite layers to form modified bentonite combined by covalent bonds, ionic bonds, coupling bonds or Van der Waals forces, and obtaining a modified bentonite suspension;
3) continuously stirring the modified bentonite suspension obtained in the step 2) for a preset time, then carrying out solid-liquid separation in a suction filtration mode, and removing filtrate to obtain a solid;
4) continuously washing the solid obtained in the step 3) with ultrapure water until the redundant quaternary phosphonium salt surfactant is completely washed away;
5) putting the solid washed by the ultrapure water in the step 4) into an oven for drying to obtain a quaternary phosphonium salt modified high-temple bentonite solid;
6) grinding the quaternary phosphonium salt modified high-temple bentonite solid into powder, and sieving to obtain the quaternary phosphonium salt modified high-temple bentonite;
the dosage of the quaternary phosphonium salt surfactant and the bentonite in the step 1) and the step 2) is determined according to the cation exchange capacity, namely the dosage of the quaternary phosphonium salt surfactant: 3.46 mmol-13.84 mmol of bentonite: 10 g.
3. The method of claim 2, wherein: the quaternary phosphonium salt surfactant in the step 1) is trihexyltetradecyl phosphonium chloride, tetrabutylphosphonium chloride or butyltriphenylphosphonium chloride.
4. The method of claim 2, wherein: and 2) the high temple bentonite in the step 2) is calcium-based high temple bentonite, the cation exchange capacity is 69.2mmol/100g, and the mixture is ground and sieved by a 200-mesh sieve.
5. The method of claim 2, wherein: the stirring in the step 1) and the step 2) is carried out on a constant-temperature magnetic stirrer, the temperature during stirring is 25-75 ℃, and the stirring speed is 100-900 r/min; the continuous stirring in the step 3) is carried out for a preset time of 24 h.
6. The method of claim 2, wherein: whether the excessive quaternary phosphonium salt surfactant is washed off in the step 4) is detected by 0.1mol/L silver nitrate solution, 4-6 drops of silver nitrate solution is added into the filtrate after the ultra-pure water washing, and if no white precipitate is generated, the excessive quaternary phosphonium salt surfactant is washed off.
7. The method of claim 2, wherein: the drying temperature in the step 5) is 60 ℃.
8. The method of claim 2, wherein: the sieving in the step 6) is 200-mesh sieving.
9. The use of the quaternary phosphonium salt modified homo temple bentonite as in claim 1, wherein: the modified quaternary phosphonium salt modified high temple bentonite is used as an adsorbent to remove iodide ions in wastewater; the dosage of the adsorbent in the wastewater is 1-10g/L, the initial concentration of iodide ions is 0.85-4.23mgmg/L, the oscillation time is 2-24h, and the temperature is 25-65 ℃.
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Application publication date: 20200915 |