CN111229158A - Preparation method of novel adsorbent for removing heavy metal antimony in water and adsorbent - Google Patents
Preparation method of novel adsorbent for removing heavy metal antimony in water and adsorbent Download PDFInfo
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 94
- 239000003463 adsorbent Substances 0.000 title claims abstract description 82
- 229910052787 antimony Inorganic materials 0.000 title claims abstract description 69
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 229910001385 heavy metal Inorganic materials 0.000 title claims abstract description 25
- 239000002808 molecular sieve Substances 0.000 claims abstract description 40
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 40
- UNJPQTDTZAKTFK-UHFFFAOYSA-K cerium(iii) hydroxide Chemical compound [OH-].[OH-].[OH-].[Ce+3] UNJPQTDTZAKTFK-UHFFFAOYSA-K 0.000 claims abstract description 38
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 23
- 229910004664 Cerium(III) chloride Inorganic materials 0.000 claims abstract description 22
- 238000001035 drying Methods 0.000 claims abstract description 14
- 238000000227 grinding Methods 0.000 claims abstract description 8
- 238000007873 sieving Methods 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000011068 loading method Methods 0.000 claims abstract description 7
- 238000000967 suction filtration Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 238000002791 soaking Methods 0.000 claims abstract description 3
- 239000007788 liquid Substances 0.000 claims description 14
- 239000000843 powder Substances 0.000 claims description 13
- 230000010355 oscillation Effects 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 238000005470 impregnation Methods 0.000 claims description 8
- 238000009210 therapy by ultrasound Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 2
- 238000012216 screening Methods 0.000 claims 1
- 238000001179 sorption measurement Methods 0.000 abstract description 49
- 230000008569 process Effects 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 30
- 239000000243 solution Substances 0.000 description 26
- 238000012360 testing method Methods 0.000 description 23
- TXTQARDVRPFFHL-UHFFFAOYSA-N [Sb].[H][H] Chemical compound [Sb].[H][H] TXTQARDVRPFFHL-UHFFFAOYSA-N 0.000 description 20
- ZDINGUUTWDGGFF-UHFFFAOYSA-N antimony(5+) Chemical compound [Sb+5] ZDINGUUTWDGGFF-UHFFFAOYSA-N 0.000 description 17
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 12
- 238000001514 detection method Methods 0.000 description 10
- 230000000694 effects Effects 0.000 description 10
- 239000011521 glass Substances 0.000 description 10
- 239000000706 filtrate Substances 0.000 description 6
- 238000009616 inductively coupled plasma Methods 0.000 description 6
- 239000012528 membrane Substances 0.000 description 6
- 229910052684 Cerium Inorganic materials 0.000 description 4
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- UCXOJWUKTTTYFB-UHFFFAOYSA-N antimony;heptahydrate Chemical compound O.O.O.O.O.O.O.[Sb].[Sb] UCXOJWUKTTTYFB-UHFFFAOYSA-N 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052700 potassium Inorganic materials 0.000 description 3
- 239000011591 potassium Substances 0.000 description 3
- 238000003723 Smelting Methods 0.000 description 2
- 229940026189 antimony potassium tartrate Drugs 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- WBTCZEPSIIFINA-MSFWTACDSA-J dipotassium;antimony(3+);(2r,3r)-2,3-dioxidobutanedioate;trihydrate Chemical compound O.O.O.[K+].[K+].[Sb+3].[Sb+3].[O-]C(=O)[C@H]([O-])[C@@H]([O-])C([O-])=O.[O-]C(=O)[C@H]([O-])[C@@H]([O-])C([O-])=O WBTCZEPSIIFINA-MSFWTACDSA-J 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000005065 mining Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000004677 Nylon Substances 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- FAWGZAFXDJGWBB-UHFFFAOYSA-N antimony(3+) Chemical compound [Sb+3] FAWGZAFXDJGWBB-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 239000004848 polyfunctional curative Substances 0.000 description 1
- IIQJBVZYLIIMND-UHFFFAOYSA-J potassium;antimony(3+);2,3-dihydroxybutanedioate Chemical compound [K+].[Sb+3].[O-]C(=O)C(O)C(O)C([O-])=O.[O-]C(=O)C(O)C(O)C([O-])=O IIQJBVZYLIIMND-UHFFFAOYSA-J 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000003828 vacuum filtration Methods 0.000 description 1
- 239000002349 well water Substances 0.000 description 1
- 235000020681 well water Nutrition 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
- B01J20/18—Synthetic zeolitic molecular sieves
- B01J20/186—Chemical treatments in view of modifying the properties of the sieve, e.g. increasing the stability or the activity, also decreasing the activity
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
Abstract
The invention discloses a preparation method of a novel adsorbent for removing heavy metal antimony in water and the adsorbent. A preparation method of a novel adsorbent for removing heavy metal antimony in water comprises the following steps: dissolving cerous chloride; adjusting the pH value; adding a Y-type molecular sieve; soaking and loading at constant temperature; carrying out suction filtration and washing; drying to constant weight; a step of cooling; grinding and sieving. The preparation method of the invention has simple operation process and low price of raw materials, and the prepared Y-shaped molecular sieve loaded cerium hydroxide type adsorbent has larger adsorption capacity to antimony in water, is suitable for antimony-containing water with different pH values, and has higher selectivity to antimony. The Y-type molecular sieve loaded cerium hydroxide adsorbent can be effectively used for treating antimony-containing water, and is a new technology worthy of vigorous popularization.
Description
Technical Field
The invention relates to the technical field of water treatment, in particular to a preparation method of a novel adsorbent for removing heavy metal antimony in water and a Y-type molecular sieve loaded cerium hydroxide type adsorbent, and particularly relates to a preparation method of a Y-type molecular sieve loaded cerium hydroxide type adsorbent for removing antimony in water.
Background
Antimony, an important industrial resource, is the 9 th metal of world's production, with global annual production exceeding 1.0 x 105t. Antimony and its compounds are useful as flame retardants, semiconductor and alloy hardeners, etc., and are closely related to human production activities. The loss of volcanic eruption, mining, metal smelting and other natural or artificial factors into the environment can cause the loss of the volcanic eruption, the mining, the metal smelting and other natural or artificial factors, the average concentration of antimony in rivers in the world is below 1 mu g/L, but the concentration of antimony in some water bodies can be as high as 30 mg/L. As the largest antimony reserves and producing countries, China faces serious antimony pollution, especially in antimony mine areas of tin mines in Hunan province, the antimony contents in the peripheral river water and well water are 1.33-21.79 mg/L and 0.037-0.063 mg/L respectively. Antimony exists mainly in the form of trivalent antimony (expressed as antimony (iii)) and pentavalent antimony (expressed as antimony (v)) in water, but antimony (iii) is more than 10 times as toxic as antimony (v). Antimony is a carcinogenic element and seriously threatens human health. Therefore, the development of a method for economically and efficiently removing antimony from water has become the current of protecting the living environment of human beingsUrgent business.
Adsorption is one of the most effective options for removing low concentrations of antimony from water. The adsorption method has the advantages of simple and quick operation, low energy consumption and the like. The existing particle adsorbents have good adsorption performance on antimony in water, but have the problems of complex preparation process and low specificity. Therefore, it is necessary to develop an adsorbent having a simple preparation process and specific adsorption properties to antimony in water.
Therefore, it is highly desirable to provide a method for preparing a novel adsorbent for removing heavy metal antimony from water, so as to remove heavy metal antimony from water with high efficiency.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, provides a preparation method of a novel adsorbent for removing heavy metal antimony in water and the prepared adsorbent, and particularly provides a Y-type molecular sieve loaded cerium hydroxide type adsorbent for removing antimony in water, which can effectively remove heavy metal antimony in water.
In order to achieve the purpose, the invention adopts the following technical scheme.
The invention provides a preparation method of a novel adsorbent for removing heavy metal antimony in water, which comprises the following steps: dissolving cerous chloride; adjusting the pH value; adding a Y-type molecular sieve; soaking and loading at constant temperature; carrying out suction filtration and washing; drying to constant weight; a step of cooling; grinding and sieving.
Further, the step of dissolving the cerous chloride is as follows: and adding deionized water into the cerous chloride powder, and performing ultrasonic treatment until the cerous chloride is completely dissolved to obtain a cerous chloride solution.
Further, the pH is adjusted to be: adjusting the pH to above 10.
Further, the pH is adjusted to be: the pH was adjusted to above 10 using sodium hydroxide.
Further, the concentration of the sodium hydroxide is 0.1-2.0 mol/L.
Further, the constant-temperature impregnation and loading steps are as follows: after the Y-type molecular sieve is added, the mixture is placed in a constant-temperature water bath oscillation container with the temperature of 25 ℃ and the rotating speed of 200r/min for impregnation reaction, so that cerium hydroxide is successfully loaded on the Y-type molecular sieve.
Further, the temperature of drying is not more than 100 ℃.
Further, the cooling step is as follows: cooled to room temperature in a desiccator.
Further, the mesh number of the sieve is 100 meshes.
Further, the mass fraction of the cerous chloride in the cerous chloride powder is 0.2-1.0%.
Further, the solid-liquid ratio of the adding amount of the Y-type molecular sieve is 1:50 (m/V).
Further, the constant-temperature impregnation time is not less than 4 h.
The invention also provides a Y-type molecular sieve loaded cerium hydroxide type adsorbent prepared by the preparation method of the novel adsorbent for removing heavy metal antimony in water.
In the invention, the Y-type molecular sieve loaded cerium hydroxide type adsorbent is used for removing heavy metal antimony in a water body.
In the invention, the application method of the Y-type molecular sieve loaded cerium hydroxide type adsorbent can be as follows: and fully contacting the Y-type molecular sieve loaded cerium hydroxide type adsorbent with antimony-containing water, adsorbing antimony in the adsorbent, and filtering to separate the antimony-containing adsorbent.
In a specific embodiment of the invention, the preparation method of the novel adsorbent for removing heavy metal antimony in water comprises the following steps:
(1) dissolving cerous chloride:
placing 0.2-1.0 mass percent of cerium chloride powder (analytically pure) into a reaction bottle filled with deionized water, placing the reaction bottle into an ultrasonic wave dissolving instrument, and performing ultrasonic treatment until the cerium chloride is completely dissolved to obtain a cerium chloride solution;
(2) adjusting the pH value:
adjusting the pH value of the cerous chloride solution to be more than 10 by using sodium hydroxide with the concentration of 0.1-2.0 mol/L;
(3) adding a Y-type molecular sieve:
after the pH value is adjusted, adding a Y-type molecular sieve to obtain a mixed liquid;
(4) constant-temperature impregnation and loading:
placing the reaction vessel filled with the mixed liquid in the step (3) in a constant-temperature water bath oscillation box for carrying out impregnation reaction, wherein the reaction temperature is 25 ℃, and the rotating speed is 200r/min, so that cerium hydroxide is successfully loaded on the Y-type molecular sieve;
(5) and (3) suction filtration and washing:
carrying out vacuum filtration on the mixed liquid obtained in the step (4), washing filter residues with deionized water for three times, and collecting the filter residues into a culture dish;
(6) drying:
drying the culture dish with the filter residue in the step (5) to constant weight, wherein the drying temperature is not more than 100 ℃;
(7) grinding and sieving:
and (4) cooling the dried solid in the step (6) to room temperature in a dryer, grinding, sieving by a 100-mesh sieve, and storing the sieved substance in the dryer to be used as an adsorbent for later use.
In the present invention, the materials used are commercially available products unless otherwise specified.
In the invention, the Y-type molecular sieve loaded cerium hydroxide type adsorbent can be used for effectively treating antimony-containing water bodies under different pH conditions. For example, the pH may be 2.0, 3.0, 4.0, 5.0, 6.0, 7.0, 8.0, 9.0, 10.0.
In the embodiment of the invention, the calculation formula of the adsorption capacity is
In the formula: q is the adsorption capacity (mg/g), C0、C1The antimony concentrations (mg/L) in the initial and post-reaction liquids, respectively, m is the amount of adsorbent added (g) and V is the volume of the solution (L).
The invention has the beneficial effects that:
according to the invention, the Y-type molecular sieve is combined with the rare earth element cerium to prepare the Y-type molecular sieve loaded cerium hydroxide adsorbent for removing antimony in water, so that the excellent structural characteristics of the Y-type molecular sieve are fully utilized, and the specific adsorption of cerium to antimony is exerted. The Y-type molecular sieve is an aluminosilicate framework structure with cubic lattice, has a larger space volume and a 3-dimensional 12-membered ring channel system, and has excellent hydrothermal stability, acid resistance and high surface polarity.
The method uses the Y-type molecular sieve loaded cerium hydroxide type adsorbent to remove the antimony in the water, has high capacity of adsorbing the antimony in the water, and has no release of cerium and no secondary pollution in the whole process. According to the experiment of the invention, when the adding amount of the adsorbent is 1g/L, the removal rate of the low-concentration (<5mg/L) antimony (III) in water is higher than 77%, and the removal rate of the low-concentration (<5mg/L) antimony (V) in water is higher than 64%, and the adsorbent has a remarkable effect on removing the antimony in the water.
The method has the advantages of simple operation process, low raw material price and larger adsorption capacity for antimony in water. The Y-type molecular sieve loaded cerium hydroxide adsorbent has high selectivity on antimony, can be used for effectively treating antimony-containing water bodies with different pH values, and is a new technology worthy of great popularization.
Drawings
In order to more clearly illustrate the technical solutions in 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 creative efforts.
FIG. 1 is a flow chart of the preparation method of the novel adsorbent for removing heavy metal antimony in water.
Detailed Description
The technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The embodiment provides a preparation method of a novel adsorbent for removing heavy metal antimony in water, and with reference to fig. 1, the preparation method comprises the following steps:
(1) dissolving cerous chloride
Weighing cerium chloride powder (analytically pure) with the mass of 0.2000g, placing the cerium chloride powder into a 250mL glass conical flask, then adding 100mL deionized water, placing the conical flask into an ultrasonic dissolver, and ultrasonically treating for 20min to completely dissolve the cerium chloride;
(2) adjusting the pH
Adjusting the pH of the solution in the conical flask in the step (1) to 10.0 by using 2.0mol/L sodium hydroxide solution;
(3) adding Y-type molecular sieve
Adding a Y-type molecular sieve (purchased from catalyst factories of southern Kai university) with the mass of 2.0000g into the mixed liquid in the step (2) according to the solid-to-liquid ratio of 1: 50;
(4) impregnation and Loading
Placing the conical flask filled with the mixed liquid in the step (3) in a constant-temperature water bath oscillation box, and reacting for 4 hours at the reaction temperature of 25 ℃ and the rotation speed of 200r/min to successfully load cerium hydroxide on the Y-type molecular sieve;
(5) suction filtration and washing
Carrying out suction filtration on the mixed solution in the step (4) by using a vacuum suction filtration pump, washing filter residues for three times by using deionized water, and collecting the filter residues into a culture dish;
(6) drying by baking
Placing the culture dish with the filter residue in the step (5) in an oven, and drying for 10 hours at 75 ℃;
(7) grinding and sieving
And (4) cooling the dried solid in the step (6) to room temperature in a dryer, grinding the cooled solid by using a ceramic mortar, sieving the ground solid by using a 100-mesh nylon standard sieve, and storing the sieved matter in the dryer to obtain the Y-type molecular sieve loaded cerium hydroxide adsorbent for later use.
1) The detection test for removing antimony (iii) in water is performed on the Y-type molecular sieve-supported cerium hydroxide type adsorbent obtained in this example, and the specific method is as follows: (test 1)
The method comprises the following steps: 0.1000g of the prepared adsorbent is weighed and placed in a 250mL glass conical flask, then 100mL of antimony (III) water with the initial concentration of 50mg/L, which is prepared from antimony potassium tartrate (analytically pure), is added into the conical flask, and then the pH value of the solution in the conical flask is adjusted to 7.0 by using a hydrochloric acid solution with the concentration of 0.1-1.0 mol/L or a sodium hydroxide solution with the concentration of 0.1-1.0 mol/L. Plugging the conical flask, placing the conical flask in a constant-temperature water bath oscillation box, carrying out adsorption reaction for 12 hours at the reaction temperature of 25 ℃ and the rotation speed of 200r/min, then, passing the liquid in the conical flask through a filter membrane of 0.45 mu m, carrying out measurement analysis on the obtained filtrate by using an inductively coupled plasma emission spectrometer, and calculating the adsorption capacity of the Y-type molecular sieve load cerium hydroxide type adsorbent without antimony (III). The test is carried out on two parallel samples, and the obtained data of the adsorption capacity is the average value of the adsorption capacities of the two parallel samples.
The detection result of the test 1 shows that: the adsorption capacity of the Y-type molecular sieve-supported cerium hydroxide adsorbent prepared by the preparation method of example 1 on antimony (III) in water was 15.68 mg/g.
2) The detection test for removing antimony (v) in water was performed on the Y-type molecular sieve-supported cerium hydroxide type adsorbent obtained in this example, and the specific method was as follows: (Note as test 2)
The method comprises the following steps: 0.1000g of the prepared adsorbent is weighed and placed in a 250mL glass reaction flask, then 100mL of antimony-containing water with the initial concentration of 50mg/L of antimony (V) prepared from potassium pyroantimonate (analytically pure) is added into the conical flask, and then the pH value of the solution in the conical flask is adjusted to 7.0 by using a hydrochloric acid solution with the concentration of 0.1-1.0 mol/L or a sodium hydroxide solution with the concentration of 0.1-1.0 mol/L. Plugging the conical flask, placing the conical flask in a constant-temperature water bath oscillation box, carrying out adsorption reaction for 12 hours at the reaction temperature of 25 ℃ and the rotation speed of 200r/min, then, passing the liquid in the conical flask through a filter membrane of 0.45 mu m, carrying out measurement analysis on the obtained filtrate by using an inductively coupled plasma emission spectrometer, and calculating the adsorption capacity of the antimony (V) -removed Y-type molecular sieve loaded cerium hydroxide type adsorbent. The test is carried out on two parallel samples, and the obtained data of the adsorption capacity is the average value of the adsorption capacities of the two parallel samples.
The detection result of the test 2 shows that: the adsorption capacity of the Y-type molecular sieve-supported cerium hydroxide adsorbent prepared by the preparation method of example 1 on antimony (V) in water was 2.67 mg/g.
Example 2
The embodiment provides a preparation method of a novel adsorbent for removing antimony in water, which comprises the following steps:
(1) dissolving cerous chloride
Weighing cerium chloride powder (analytically pure) with the mass of 0.4000g, placing the cerium chloride powder into a 250mL glass conical flask, then adding 100mL deionized water, placing the conical flask into an ultrasonic wave dissolver, and carrying out ultrasonic treatment for 20min to completely dissolve the cerium chloride;
(2) steps (1) to (7) were the same as in example 1.
The detection test for removing antimony in water was performed on the Y-type molecular sieve-supported cerium hydroxide type adsorbent obtained in this example, and the detection method was the same as in example 1:
the detection result of the present example shows that: the adsorption capacity of the Y-type molecular sieve-loaded cerium hydroxide adsorbent prepared in the embodiment 2 of the invention on antimony (III) in water is 23.06mg/g, and the adsorption capacity on antimony (V) in water is 7.18 mg/g.
Example 3
The embodiment provides a preparation method of a novel adsorbent for removing antimony in water, which comprises the following steps:
(1) dissolving cerous chloride
Weighing 1.0000g of cerous chloride powder (analytically pure) by mass, placing the cerous chloride powder into a 250mL glass conical flask, then adding 100mL deionized water, placing the conical flask into an ultrasonic dissolver, and carrying out ultrasonic treatment for 20min to completely dissolve the cerous chloride. (ii) a
(2) Steps (1) to (7) were the same as in example 1.
The detection test for removing antimony in water was performed on the Y-type molecular sieve-supported cerium hydroxide type adsorbent obtained in this example, and the detection method was the same as in example 1:
the detection result of the present example shows that: the adsorption capacity of the Y-type molecular sieve-supported cerium hydroxide adsorbent prepared under the preparation method of example 3 on antimony (III) in water was 30.96mg/g, and the adsorption capacity on antimony (V) in water was 11.89 mg/g.
Example 4
A preparation method of a novel adsorbent for removing antimony in water comprises the following steps:
(1) dissolving cerous chloride
Weighing cerium chloride powder (analytically pure) with the mass of 0.4000g, placing the cerium chloride powder into a 250mL glass conical flask, then adding 100mL deionized water, placing the conical flask into an ultrasonic dissolver, and carrying out ultrasonic treatment for 20min to completely dissolve the cerium chloride.
(2) Steps (1) to (5) are the same as in example 1
(6) Drying by baking
Placing the culture dish with the filter residue in the step (5) in an oven, and drying at 80 ℃ for 10 h;
(7) grinding and sieving (same as example 1)
1) The effect of the Y-type molecular sieve-supported cerium hydroxide adsorbent obtained in this example on removing antimony (iii) in water was tested: (test 3)
The method comprises the following steps: 0.1000g of the prepared adsorbent is weighed into 3 250mL glass conical flasks, 100mL of antimony (III) containing water with initial concentrations of 5, 25 and 50mg/L, which is prepared from potassium antimony tartrate (analytically pure), is added into the conical flasks, and the pH of the solution in 3 conical flasks is adjusted to 7.0 by using a hydrochloric acid solution with a concentration of 0.1-1.0 mol/L or a sodium hydroxide solution with a concentration of 0.1-1.0 mol/L. Plugging each conical flask, placing the conical flask in a constant-temperature water bath oscillation box, carrying out adsorption reaction for 12 hours at the reaction temperature of 25 ℃ and the rotation speed of 200r/min, respectively passing the liquid in the conical flask through 0.45-micrometer filter membranes, measuring and analyzing the obtained filtrate by using an inductively coupled plasma emission spectrometer, and respectively calculating the adsorption capacity of the Y-type molecular sieve load cerium hydroxide type adsorbent for removing antimony (III). The test is carried out on two parallel samples, and the obtained data of the adsorption capacity is the average value of the adsorption capacities of the two parallel samples. The results of test 3 are shown in Table 1.
TABLE 1
| Initial concentration (mg/L) of antimony (III) | 5 | 25 | 50 |
| Adsorption capacity (mg/g) | 3.89 | 14.93 | 21.64 |
| Removal ratio of antimony (III) (%) | 77.8 | 59.7 | 43.3 |
As can be seen from the test data shown in Table 1, ① shows that the adsorption capacity of the adsorbent to antimony (III) does not change much when the drying temperature is increased from 75 ℃ to 80 ℃ compared with that of example 2, and ② shows that the removal rate of antimony (III) at a low concentration (<5mg/L) in water is higher than 77% when the addition amount of the adsorbent is 1 g/L.
2) The effect of the Y-type molecular sieve-supported cerium hydroxide type adsorbent obtained in this example on removing antimony (v) in water was tested: (test 4)
The method comprises the following steps: 0.1000g of the prepared adsorbent is weighed into 3 250mL glass conical flasks, 100mL of antimony-containing water with initial antimony (V) concentrations of 5, 25 and 50mg/L, which is prepared from potassium pyroantimonate (analytically pure), is added into the conical flasks, and then the pH of the solution in the 3 conical flasks is adjusted to 7.0 by using 0.1-1.0 mol/L hydrochloric acid solution or 0.1-1.0 mol/L sodium hydroxide solution. Plugging each conical flask, placing the conical flask in a constant-temperature water bath oscillation box, carrying out adsorption reaction for 12 hours at the reaction temperature of 25 ℃ and the rotation speed of 200r/min, respectively passing the liquid in the conical flask through 0.45-micrometer filter membranes, measuring and analyzing the obtained filtrate by using an inductively coupled plasma emission spectrometer, and respectively calculating the adsorption capacity of the antimony (V) -removed Y-type molecular sieve loaded cerium hydroxide type adsorbent. Two parallel samples were made for this test, and the data obtained for adsorption capacity was the average of the adsorption capacities of the two parallel samples. The results of test 4 are shown in Table 2.
TABLE 2
| Initial concentration (mg/L) of antimony (V) | 5 | 25 | 50 |
| Adsorption capacity (mg/g) | 3.20 | 4.66 | 7.39 |
| Removal ratio of antimony (V) (%) | 64.0 | 18.6 | 14.8 |
As can be seen from the data in Table 2, ① shows that the adsorption capacity of the adsorbent to antimony (V) does not change much when the drying temperature is increased from 75 deg.C to 80 deg.C as compared with example 2, and ② shows that the removal rate of antimony (V) at a low concentration (<5mg/L) in water is higher than 64% when the addition amount of the adsorbent is 1 g/L.
3) The effect of the Y-type molecular sieve-supported cerium hydroxide adsorbent obtained in this example on removing antimony (iii) in water was tested: (test 5)
The method comprises the following steps: 0.1000g of the prepared adsorbent is weighed into 6 250mL glass conical flasks, 100mL of antimony (III) containing water with the initial concentration of 35mg/L, which is prepared from antimony potassium tartrate (analytically pure), is added into each conical flask, and then the pH of the solution in the 6 conical flasks is adjusted to 2.0, 3.0, 4.0, 5.0, 6.0 and 7.0 by using a hydrochloric acid solution with the concentration of 0.1-1.0 mol/L or a sodium hydroxide solution with the concentration of 0.1-1.0 mol/L. Plugging each conical flask, placing the conical flask in a constant-temperature water bath oscillation box, carrying out adsorption reaction for 12 hours at the reaction temperature of 25 ℃ and the rotation speed of 200r/min, respectively passing the liquid in the conical flask through 0.45-micrometer filter membranes, measuring and analyzing the obtained filtrate by using an inductively coupled plasma emission spectrometer, and respectively calculating the adsorption capacity of the Y-type molecular sieve load cerium hydroxide type adsorbent for removing antimony (III). The test is carried out on two parallel samples, and the obtained data of the adsorption capacity is the average value of the adsorption capacities of the two parallel samples. The results of test 5 are shown in Table 3.
TABLE 3
| Initial pH | 2.0 | 3.0 | 4.0 | 5.0 | 6.0 | 7.0 |
| Adsorption capacity (mg/g) | 30.80 | 33.15 | 27.25 | 24.85 | 21.3 | 19.75 |
From the data in table 3, it can be seen that: the Y-type molecular sieve-supported cerium hydroxide-type adsorbent prepared under the preparation method of example 4 has a good adsorption effect on antimony (iii) in water at different initial pH values, and has a better adsorption effect at an initial pH value of 3.
4) The effect of the Y-type molecular sieve-supported cerium hydroxide type adsorbent obtained in this example on removing antimony (v) in water was tested: (test 6)
The method comprises the following steps: 0.1000g of the prepared adsorbent is weighed into 9 250mL glass conical flasks, 100mL of antimony-containing water with the initial concentration of 35mg/L and prepared from potassium pyroantimonate (analytically pure) is added into each conical flask, and then the pH of the solution in the 9 conical flasks is respectively adjusted to 2.0, 3.0, 4.0, 5.0, 6.0, 7.0, 8.0, 9.0 and 10.0 by using a hydrochloric acid solution with the concentration of 0.1-1.0 mol/L or a sodium hydroxide solution with the concentration of 0.1-1.0 mol/L. Plugging each conical flask, placing the conical flask in a constant-temperature water bath oscillation box, carrying out adsorption reaction for 12 hours at the reaction temperature of 25 ℃ and the rotation speed of 200r/min, then, filtering liquid in the conical flask through a filter membrane of 0.45 mu m, carrying out measurement and analysis on the obtained filtrate by using an inductively coupled plasma emission spectrometer, and respectively calculating the adsorption capacity of the Y-type molecular sieve load cerium hydroxide type adsorbent for removing antimony (V). The test is carried out on two parallel samples, and the obtained data of the adsorption capacity is the average value of the adsorption capacities of the two parallel samples. The results of test 6 are shown in Table 4.
TABLE 4
| Initial pH | 2.0 | 3.0 | 4.0 | 5.0 | 6.0 | 7.0 | 8.0 | 9.0 | 10.0 |
| Adsorption capacity (mg/g) | 8.55 | 5.95 | 6.25 | 6.15 | 5.95 | 6.05 | 5.95 | 5.85 | 4.15 |
From the data in table 4, it can be seen that: the Y-type molecular sieve-supported cerium hydroxide type adsorbent prepared under the preparation method of example 4 has a better adsorption effect on antimony (v) in water at different initial pH values, and the adsorption effect is better when the initial pH value is 2.0.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The preparation method of the novel adsorbent for removing heavy metal antimony in water is characterized by comprising the following steps of: dissolving cerous chloride; adjusting the pH value; adding a Y-type molecular sieve; soaking and loading at constant temperature; carrying out suction filtration and washing; drying to constant weight; a step of cooling; grinding and sieving.
2. The method for preparing the novel adsorbent for removing the heavy metal antimony in water according to claim 1, wherein the step of dissolving the cerous chloride is as follows: and adding deionized water into the cerous chloride powder, and performing ultrasonic treatment until the cerous chloride is completely dissolved to obtain a cerous chloride solution.
3. The method for preparing the novel adsorbent for removing the heavy metal antimony in water according to claim 1, wherein the pH is adjusted to be: adjusting the pH to above 10.
4. The preparation method of the novel adsorbent for removing the heavy metal antimony in water according to claim 1, wherein the constant-temperature impregnation and loading steps are as follows: after the Y-type molecular sieve is added, the mixture is placed in a constant-temperature water bath oscillation container with the temperature of 25 ℃ and the rotating speed of 200r/min for impregnation reaction, so that cerium hydroxide is loaded on the Y-type molecular sieve.
5. The method for preparing the novel adsorbent for removing the heavy metal antimony in water according to claim 2, wherein the mass fraction of the cerium chloride powder is 0.2-1.0%.
6. The preparation method of the novel adsorbent for removing the heavy metal antimony in water according to claim 1 or 4, wherein the Y-type molecular sieve is added in a solid-to-liquid ratio of 1: 50.
7. the method for preparing the novel adsorbent for removing the heavy metal antimony in water according to claim 1, wherein the drying temperature is not more than 100 ℃.
8. The method for preparing the novel adsorbent for removing the heavy metal antimony in water according to claim 1, wherein the cooling step comprises: cooled to room temperature in a desiccator.
9. The method for preparing the novel adsorbent for removing the heavy metal antimony in water according to claim 1, wherein the screening mesh number is 100 meshes.
10. The Y-type molecular sieve-loaded cerium hydroxide adsorbent is characterized by being prepared by the preparation method of the novel adsorbent for removing heavy metal antimony in water according to any one of claims 1 to 9.
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