CN112742344A - Preparation method of ZnFe-LDHs/diatomite composite material - Google Patents
Preparation method of ZnFe-LDHs/diatomite composite material Download PDFInfo
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- CN112742344A CN112742344A CN202011472696.XA CN202011472696A CN112742344A CN 112742344 A CN112742344 A CN 112742344A CN 202011472696 A CN202011472696 A CN 202011472696A CN 112742344 A CN112742344 A CN 112742344A
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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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Abstract
The invention discloses a preparation method of ZnFe-LDHs/diatomite composite material, which comprises the steps of activating and modifying diatomite in an acidic activation, roasting activation or microwave activation mode, removing bound water, sodium, potassium and other impurities in the diatomite to increase the pore space and the specific surface area of the diatomite, wherein the modified diatomite has rich pore structure, and ZnFe-LDHs is attached to the surface and the macropores of the diatomite to greatly improve the fluorine adsorption capacity of the material; in addition, the surface of the obtained composite material is modified by using an anionic surfactant, structural water and non-bridging hydroxyl groups among ZnFe-LDHs layers are eliminated, the steric hindrance among particles is enhanced, the lap joint among the particles is prevented, and the adsorption performance of fluorine is improved. In the prepared composite material, ZnFe-LDHs is attached to the surface and the coarse pores of the diatomite, the pore structure of the diatomite is completely reserved, the fluorine adsorption capacity of the integral material is improved through the attached ZnFe-LDHs while the fluorine adsorption capacity of the diatomite is ensured, and the problem that the pure ZnFe-LDHs is difficult to filter is solved.
Description
Technical Field
The invention relates to the technical field of zinc hydrometallurgy, in particular to a preparation method of a ZnFe-LDHs/diatomite composite material.
Background
Along with the continuous exploitation of mineral resources, zinc ores tend to be poor, fine and impure, so that zinc concentrate produced by flotation is low in grade and high in impurity content, and particularly the fluorine content is higher and higher. In the zinc smelting process, the cathode aluminum plate can be corroded due to too high concentration of fluorine ions in the electrolyte, the passive film on the cathode plate is damaged, so that the separated zinc and the aluminum plate are adhered, the zinc stripping is difficult, the consumption of the cathode plate is increased, and the electrolytic process can not be normally carried out. In addition, fluorine accelerates corrosion of steel members, increases wear of equipment such as pumps and mixers, and increases production costs. Therefore, the development of a technology for efficiently removing fluorine in a zinc smelting system is urgently needed.
Layered composite metal hydroxides (LDHs) are novel inorganic functional materials with a supermolecular intercalation structure, and the general formula of the composition can be expressed as follows: [ M ] A1-x 2+Mx 3+(OH)2]x+(An -)x/n·mH2O, wherein M2+And M3+Respectively representing divalent and trivalent metal cations, e.g. Mg2+、Zn2+、Ca2+、Co2+、Fe2+With Al3+、Ga3+、Fe3+、Cr3+And the like. LDHs can remove inorganic or organic anions by ion exchange and surface adsorption based on their unique compositions and layered structures. However, most of the existing LDHs are Mg-Al, Ca-Al and Mg-Fe types, impurities are easy to introduce into a zinc smelting system, and the LDHs are nano or micron powder, so that solid-liquid separation is difficult in actual use, and secondary pollution is easy to cause.
Diatomite is a siliceous rock and has the characteristics of rich pore structure, stable chemical property and the like. However, a large amount of impurities are adhered to the internal structure of the common diatomite, so that the adhesion vacancy of the diatomite is occupied, the surface area of the diatomite is reduced, fluorine ions are prevented from entering the structure of the diatomite, the adsorption capacity of fluorine is low, and the application of the diatomite in fluorine adsorption is limited.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method of a ZnFe-LDHs/diatomite composite material, which takes modified diatomite as a carrier to synthesize a zinc-iron layered composite metal hydroxide/diatomite composite material for cleaning a zinc smelting system and realize the efficient removal of fluorine in the zinc smelting system.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a ZnFe-LDHs/diatomite composite material comprises the following steps:
s1, acidifying and modifying the diatomite: placing diatomite in a beaker, adding a sulfuric acid solution with a liquid-solid ratio of 4-10:1 and a sulfuric acid concentration of 0.2-1.1mol/L, stirring for 4-8h at the temperature of 40-70 ℃, filtering, washing the obtained diatomite with clear water until the washing water is neutral, and then air-drying to constant weight; the liquid-solid ratio is the volume-mass ratio;
s2, roasting and activating or microwave activating the acidified and modified diatomite obtained in the step S1, wherein the roasting temperature is 350-550 ℃, and the roasting time is 2-3 h; when microwave activation is adopted, the microwave frequency is 3500-4000MHz, and the heating time is 25 min;
s3, preparing a zinc-iron mixed solution from zinc salt and iron salt, wherein the mass concentrations of the zinc salt and the iron salt are 0.4-6% respectively;
s4, preparation of ZnFe-LDHs/diatomite composite material: mixing the diatomite activated in the step S2 with a zinc-iron mixed solution according to a solid-to-liquid ratio of 1:50-300, adjusting the pH to 7-9, and carrying out a coprecipitation reaction under the reaction conditions of 40-60 ℃ and 1.5-3h, wherein the generated ZnFe-LDHs are attached to the surface and large pores of the diatomite; after the reaction is completed, carrying out aging, carrying out solid-liquid separation after aging, wherein the aging time is 4-6h, and the aging temperature is 100-125 ℃; the solid-liquid ratio is a mass-volume ratio;
s5, carrying out surface modification on the solid obtained by solid-liquid separation in the step S4, adding an anionic surfactant according to 0.5-3% of the mass of the solid, using water as a solvent, modifying for 1.5-3h at the temperature of 30-60 ℃ at the liquid-solid ratio of 4-7:1, filtering, washing the filtered solid with clear water until the washing water is neutral, and drying to obtain the ZnFe-LDHs/diatomite composite material; the liquid-solid ratio is a volume-mass ratio.
Further, the zinc salt is one or more of zinc nitrate, zinc sulfate and zinc acetate.
Further, the iron salt is one or more of ferric nitrate, ferric sulfate and ferric acetate.
Further, in step S4, a pH adjusting agent is used to adjust the pH, and the pH adjusting agent is one of sodium hydroxide, ammonia water, and urea.
Further, in step S4, ultrasonic waves are used to enhance precipitation during the coprecipitation reaction, and the ultrasonic power is 40W.
Further, in step S5, one or more of sodium stearate, potassium stearate, ammonium stearate, methacrylic acid, and acrylic acetate is used as the anionic surfactant.
The invention has the beneficial effects that:
1. the method of the invention firstly provides and successfully prepares the ZnFe-LDHs/kieselguhr composite material, the adsorbent has the advantages of high fluorine adsorption capacity, easy separation and no pollution, and overcomes the defects that LDHs fine particles are difficult to filter and easy to cause secondary pollution and the kieselguhr fluorine adsorption capacity is low.
2. The ZnFe-LDHs prepared by the method is used for removing fluorine in a zinc smelting system, and can avoid the introduction of impurities such as Mg, Al, Ca and the like compared with MgAl-LDHs, CaAl-LDHs and the like.
3. According to the method, the diatomite is activated and modified by adopting a mode of acid activation, roasting activation or microwave activation, bound water, sodium, potassium and other impurities in the diatomite are removed, so that the pore space and the specific surface area of the diatomite are increased, the modified diatomite has a rich pore structure, and ZnFe-LDHs is attached to the surface and the large pore space of the diatomite, so that the fluorine adsorption capacity of the material is greatly improved;
4. according to the invention, the surface of the obtained composite material is modified by using the anionic surfactant, structural water and non-bridging hydroxyl groups among ZnFe-LDHs layers are eliminated, the steric hindrance among particles is enhanced, the overlapping among particles is prevented, and the fluorine adsorption performance is improved.
5. In the method, ZnFe-LDHs is attached to the surface and the coarse pores of the diatomite, so that the pore structure of the diatomite is completely reserved, the fluorine adsorption capacity of the integral material is improved through the attached ZnFe-LDHs while the fluorine adsorption capacity of the diatomite is ensured, and the problem that the pure ZnFe-LDHs is difficult to filter is solved.
Detailed Description
The present invention will be further described below, and it should be noted that the present embodiment is based on the technical solution, and a detailed implementation manner and a specific operation process are provided, but the protection scope of the present invention is not limited to the present embodiment.
Example 1
The embodiment provides a preparation method of a ZnFe-LDHs/diatomite composite material, which comprises the following specific steps:
(1) placing the diatomite in a beaker, adding a sulfuric acid solution, stirring for 4 hours under the conditions of a liquid-solid ratio (volume/mass) of 4:1, a solution temperature of 40 ℃ and a sulfuric acid concentration of 0.5mol/L, filtering, washing the obtained diatomite with clear water until the washing water is neutral, and then air-drying to constant weight.
(2) Roasting the acidified modified diatomite for 2 hours at the roasting temperature of 350 ℃ to obtain the roasted and activated diatomite.
(3) Zinc nitrate and ferric nitrate are utilized to prepare a zinc-iron mixed solution, and the mass concentrations of the zinc nitrate and the ferric nitrate are respectively 4% and 2%.
(4) Placing the activated diatomite in a container filled with a zinc-iron mixed solution according to a solid-to-liquid ratio (mass/volume) of 1:100, adjusting the pH to 9 by using sodium hydroxide, and carrying out coprecipitation reaction for 3 hours at a reaction temperature of 50 ℃. After the reaction is completed, the mixture is aged for 6 hours at the temperature of 105 ℃, and solid-liquid separation is carried out after the aging.
(5) Adding sodium stearate into the solid according to 1% of the solid mass obtained by solid-liquid separation, carrying out surface modification for 2h at the temperature of 40 ℃ and the liquid-solid ratio of 4:1, filtering, washing the solid with clear water until the washing water is neutral, and drying to obtain the ZnFe-LDHs/diatomite composite material.
Example 2
The embodiment provides a preparation method of a ZnFe-LDHs/diatomite composite material, which comprises the following specific steps:
(1) the diatomite is placed in a beaker for acidification modification, a sulfuric acid solution is added, the mixture is stirred for 4 hours under the conditions that the liquid-solid ratio (volume/mass) is 10:1, the solution temperature is 70 ℃, and the sulfuric acid concentration is 1.1mol/L, the mixture is filtered, and the obtained diatomite is washed by clean water until the washing water is neutral and then is dried to constant weight.
(2) Roasting the acidified modified diatomite for 3 hours at the roasting temperature of 550 ℃ to obtain roasted activated diatomite.
(3) Zinc-iron solution is prepared by utilizing zinc acetate and ferric sulfate, wherein the mass concentration of the zinc acetate and the mass concentration of the ferric sulfate are respectively 6% and 2.5%.
(4) The activated diatomite is placed in a container filled with a zinc-iron mixed solution according to the solid-to-liquid ratio (mass/volume) of 1:50, the pH value is adjusted to 8.8 by ammonia water, and the coprecipitation reaction is carried out for 2 hours at the reaction temperature of 60 ℃. After the reaction is finished, aging is carried out for 4 hours at the temperature of 125 ℃, and solid-liquid separation is carried out after aging.
(5) Adding ammonium stearate into the solid according to the mass which is 1.5 percent of the mass of the solid obtained by solid-liquid separation, using water as a solvent, carrying out surface modification for 3h at the temperature of 30 ℃ and the liquid-solid ratio (volume/mass) of 4:1, filtering, washing the solid with clear water until the washing water is neutral, and drying to obtain the ZnFe-LDHs/diatomite composite material.
Example 3
The embodiment provides a preparation method of a ZnFe-LDHs/diatomite composite material, which comprises the following specific steps:
(1) placing the diatomite in a beaker, adding a sulfuric acid solution, stirring for 6 hours under the conditions of a liquid-solid ratio (volume/mass) of 8:1, a solution temperature of 60 ℃ and a sulfuric acid concentration of 0.3mol/L, filtering, washing the obtained diatomite with clear water until the washing water is neutral, and then air-drying to constant weight.
(2) And (3) activating the acidified modified diatomite for 25min at the microwave frequency of 4000MHz to obtain the microwave activated diatomite.
(3) Zinc sulfate and ferric nitrate are used for preparing a zinc-iron solution, and the mass concentrations of the zinc sulfate and the ferric nitrate are 0.8 percent and 0.4 percent respectively.
(4) The activated and modified diatomite is placed in a container filled with a zinc-iron mixed solution according to the solid-to-liquid ratio (mass/volume) of 1:200, the pH value is adjusted to 8 by utilizing urea, and the coprecipitation reaction is carried out for 3 hours at the reaction temperature of 50 ℃. After the reaction is finished, aging is carried out for 4 hours at the temperature of 125 ℃, and solid-liquid separation is carried out after aging.
(5) Adding methacrylic acid into the solid according to 0.5 percent of the mass of the solid obtained by solid-liquid separation, carrying out surface modification for 2h at the temperature of 60 ℃ and the liquid-solid ratio (volume/mass) of 5:1, filtering, washing the solid with clear water until the washing water is neutral, and drying to obtain the ZnFe-LDHs/diatomite composite material.
Example 4
The embodiment provides a preparation method of a ZnFe-LDHs/diatomite composite material, which comprises the following specific steps:
(1) placing the diatomite in a beaker, adding a sulfuric acid solution, stirring for 8 hours under the conditions of a liquid-solid ratio of 5:1, a solution temperature of 50 ℃ and a sulfuric acid concentration of 0.2mol/L, filtering, washing the obtained diatomite with clear water until the washing water is neutral, and then air-drying to constant weight.
(2) Activating the acidified modified diatomite for 25min at a microwave frequency of 3500MHz to obtain the microwave activated diatomite.
(3) Zinc nitrate and ferric acetate are used for preparing a zinc-iron solution, wherein the mass concentrations of the zinc nitrate and the ferric acetate are respectively 2% and 1%.
(4) The activated and modified diatomite is placed in a container filled with a zinc-iron mixed solution according to the solid-to-liquid ratio (mass/volume) of 1:300, the pH value is adjusted to 7 by using sodium hydroxide, and the coprecipitation reaction is carried out for 1.5h at the reaction temperature of 40 ℃ and the ultrasonic power of 40W. After the reaction is finished, aging is carried out for 5 hours at the temperature of 100 ℃, and solid-liquid separation is carried out after aging.
(5) Adding acrylic ester acetate according to 3% of the solid mass obtained by solid-liquid separation, carrying out surface modification for 1.5h at the temperature of 30 ℃ and the liquid-solid ratio (volume/mass) of 7:1, filtering, washing the solid to be neutral by using clear water, and drying to obtain the ZnFe-LDHs/diatomite composite material.
The ZnFe-LDHs/diatomite composite materials obtained in examples 1 to 4 were subjected to a zinc sulfate solution fluorine adsorption test, and the results are shown in Table 1.
TABLE 1 result of defluorination test of ZnFe-LDHs/diatomite composite material
It can be seen that the ZnFe-LDHs/diatomite composite materials prepared in the embodiments 1-4 can play an effective role in removing fluorine, and the fluorine content in the stock solution is greatly reduced after the fluorine is removed by using the composite materials.
Various corresponding changes and modifications can be made by those skilled in the art based on the above technical solutions and concepts, and all such changes and modifications should be included in the protection scope of the present invention.
Claims (7)
1. A preparation method of a ZnFe-LDHs/diatomite composite material is characterized by comprising the following steps:
s1, acidifying and modifying the diatomite: placing diatomite in a beaker, adding a sulfuric acid solution with a liquid-solid ratio of 4-10:1 and a sulfuric acid concentration of 0.2-1.1mol/L, stirring for 4-8h at the temperature of 40-70 ℃, filtering, washing the obtained diatomite with clear water until the washing water is neutral, and then air-drying to constant weight; the liquid-solid ratio is the volume-mass ratio;
s2, roasting and activating or microwave activating the acidified and modified diatomite obtained in the step S1, wherein the roasting temperature is 350-550 ℃, and the roasting time is 2-3 h; when microwave activation is adopted, the microwave frequency is 3500-4000MHz, and the heating time is 25 min;
s3, preparing a zinc-iron mixed solution from zinc salt and iron salt, wherein the mass concentrations of the zinc salt and the iron salt are 0.4-6% respectively;
s4, preparation of ZnFe-LDHs/diatomite composite material: mixing the diatomite activated in the step S2 with a zinc-iron mixed solution according to a solid-to-liquid ratio of 1:50-300, adjusting the pH to 7-9, and carrying out a coprecipitation reaction under the reaction conditions of 40-60 ℃ and 1.5-3h, wherein the generated ZnFe-LDHs are attached to the surface and large pores of the diatomite; after the reaction is completed, carrying out aging, carrying out solid-liquid separation after aging, wherein the aging time is 4-6h, and the aging temperature is 100-125 ℃; the solid-liquid ratio is a mass-volume ratio;
s5, carrying out surface modification on the solid obtained by solid-liquid separation in the step S4, adding an anionic surfactant according to 0.5-3% of the mass of the solid, using water as a solvent, modifying for 1.5-3h at the temperature of 30-60 ℃ at the liquid-solid ratio of 4-7:1, filtering, washing the filtered solid with clear water until the washing water is neutral, and drying to obtain the ZnFe-LDHs/diatomite composite material; the liquid-solid ratio is a volume-mass ratio.
2. The preparation method according to claim 1, wherein the zinc salt is one or more of zinc nitrate, zinc sulfate and zinc acetate.
3. The preparation method of claim 1, wherein the iron salt is one or more of ferric nitrate, ferric sulfate and ferric acetate.
4. The method according to claim 1, wherein in step S4, pH is adjusted by using a pH adjuster selected from one of sodium hydroxide, ammonia water, and urea.
5. The method of claim 1, wherein in step S4, ultrasonic wave is used to enhance precipitation during the coprecipitation reaction, and the ultrasonic power is 40W.
6. The method of claim 1, wherein in step S5, the anionic surfactant is one or more selected from sodium stearate, potassium stearate, ammonium stearate, methacrylic acid, and acrylic acetate.
7. The ZnFe-LDHs/diatomite composite material prepared by the preparation method of any one of the claims 1 to 6.
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| CN1792808A (en) * | 2006-01-06 | 2006-06-28 | 北京化工大学 | Inserting layer iron base hydrotalcite of negative ion type surface active agent and preparation process thereof |
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2020
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| CN1792808A (en) * | 2006-01-06 | 2006-06-28 | 北京化工大学 | Inserting layer iron base hydrotalcite of negative ion type surface active agent and preparation process thereof |
| CN101164688A (en) * | 2007-07-30 | 2008-04-23 | 山东大学 | Organic/inorganic substance layered composite functional material and preparation method thereof |
| CN104703918A (en) * | 2012-09-28 | 2015-06-10 | Scg化学有限公司 | Modification of layered double hydroxides |
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