CN118145713A - Method for preparing anhydrous ferric phosphate by reduction roasting of pyrite - Google Patents
Method for preparing anhydrous ferric phosphate by reduction roasting of pyrite Download PDFInfo
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Abstract
The invention discloses a method for preparing anhydrous ferric phosphate by utilizing pyrite reduction roasting, belongs to the technical field of pyrite treatment, and is used for solving the technical defect that valuable metal elements such as copper, gold, silver and the like are discarded in the process of preparing anhydrous ferric sulfate from pyrite cinder, so that the problem of poor adsorption efficiency of heavy metal elements is solved, and specific synthetic resin is designed to improve the adsorption efficiency; the invention comprises the following steps: the pyrite cinder reacts with ammonia water in a mixing way to obtain filtrate, namely copper ammonia mixed liquor, the solid is left for the next treatment, sulfuric acid is adopted for dissolving the solid to obtain mixed liquor, the mixed liquor is mixed with resin for adsorbing Congo red, the solid is composite resin for adsorbing Au and Ag, and the mixed liquor is subjected to heating, condensation, high-temperature roasting, deliquescence and secondary high-temperature roasting processes to prepare anhydrous ferric sulfate.
Description
Technical Field
The invention relates to the technical field of pyrite treatment, in particular to a method for preparing anhydrous ferric phosphate by utilizing pyrite reduction roasting.
Background
The pyrite is also called pyrite, the main component is ferrous disulfide (FeS 2), is the sulfide with the widest distribution in the crust, is the main raw material for preparing sulfuric acid, and can bring huge environmental problems if the part of solid waste cannot be properly treated in the case that the burned slag generated by the acid preparation of pyrite is more than ten million tons per year in China;
The material composition in the pyrite cinder is mainly iron-containing phase, the content is generally 40-60%wt, wherein the vast majority is Fe 2O3, and a small amount of Fe 3O4 phase is provided, valuable metals such as copper, lead, silver and gold and non-metal components such as SiO 2、Al2O3 are also contained in the pyrite cinder, the nonferrous metals and noble metals in the pyrite are almost all remained in the cinder, anhydrous ferric sulfate is used as a common solid drying agent, and after the anhydrous ferric sulfate absorbs water, fe 2(SO4)3·9H2O,Fe2(SO4)3·9H2 O can not lose all crystal water at the high temperature of 170-180 ℃, so that the anhydrous ferric sulfate has strong drying capability, and the anhydrous ferric phosphate prepared by the reduction roasting of the pyrite and the valuable inorganic metals in the pyrite are recovered, thereby having positive effects on realizing the full utilization of the pyrite cinder.
The invention patent CN104384171B discloses a resource recycling method of pyrite cinder, which is characterized in that the pyrite cinder is separated into aluminum hydroxide and calcium hydroxide by water suspension, carbon dioxide or sodium hydroxide and potassium hydroxide are used for reaction in water, calcium carbonate or calcium hydroxide and aluminum hydroxide or sodium aluminate and potassium aluminate are separated and recycled, ammonium bicarbonate or ammonium sulfate/ammonium chloride or phosphoric acid is used for dissolving and separating magnesium oxide, sodium hydroxide or potassium hydroxide is used for treating ferric oxide or/and waste residues of ferrous oxide, silicon dioxide and sulfur are dissolved and separated, and ferric oxide or/and ferrous oxide, silicic acid, potassium salt or sodium salt and sulfur are recovered, so that the method is applied to separation, recycling and recycling of the pyrite cinder; however, the method for recycling the resources mainly collects and separates nonmetallic components and major metallic elements, but fails to focus on selective adsorption of trace metals and nonferrous metals;
In view of the technical drawbacks of this aspect, a solution is now proposed.
Disclosure of Invention
The invention aims to provide a method for preparing anhydrous ferric phosphate by using pyrite through reduction roasting, which is used for solving the problems that a large amount of valuable heavy metal elements are wasted and the adsorption efficiency of the metal elements is low and the singleness is not strong in the preparation of anhydrous ferric sulfate by using pyrite.
The aim of the invention can be achieved by the following technical scheme: the method for preparing anhydrous ferric phosphate by utilizing pyrite through reduction roasting comprises the following steps:
S1, weighing a certain amount of pyrite cinder, crushing to 50-100 meshes, and mixing with ammonia water to obtain a mixture; heating the mixture until the heating temperature of the mixture reaches 40-50 ℃, mixing and stirring to react for 30min, and then carrying out solid-liquid separation, wherein filtrate is copper ammonia mixed solution; the filter residue is processed in the next step;
The components of pyrite cinder are mainly divided into three main categories, namely Fe 2O3/Fe3O4 phase, valuable metals such as copper, silver and gold, and non-metallic components such as SiO 2、Al2O3. The method firstly recovers copper in pyrite cinder. When ammonia water is adopted for leaching, copper and ammonia molecules can form copper ammonia complex, so that copper elements can be dissolved in the filtrate. While iron remains in the solid because it is insoluble in aqueous ammonia. In addition, heavy metal elements such as gold and silver which need to be recovered do not react with ammonia water due to the inactivity of the reaction.
S2, mixing sulfuric acid with the weight of 20% with deionized water to obtain an acidification system; mixing an acidification system and filter residues according to a solid-to-liquid ratio of 1:3, and dissolving the filter residues to obtain a mixed solution;
s3, mixing the mixed solution with the resin for adsorbing Congo red, adsorbing for 12 hours, and filtering the solid, wherein the solid is the composite resin for adsorbing Au and Ag; the filtrate is processed in the next step;
s4, mixing the filtrate with sulfuric acid to obtain a mixed solution; heating the porcelain bowl until the mixed solution is fired into a solidified material block by liquid, and cooling to room temperature; and transferring the porcelain bowl into a fume hood, and standing for 24 hours at room temperature to obtain ferric sulfate solid.
Further, the mixing amount ratio of the pyrite cinder and the ammonia water is 30g:100-150mL.
Further, the preparation method of the resin for adsorbing Congo red in the step S3 specifically comprises the following steps:
A1, mixing 100mL of deionized water and 20mL of 5%wt of ethanol to obtain a solvent; then, regulating the pH value of the mixed solution to 7-8 by using 30 wt% NaOH solution to obtain the mixed solution; stirring the mixed solution at a constant speed of 30-50r/min for 60min to obtain mother solution;
A2, adding resorcinol and melamine formaldehyde resin into the mother liquor, and uniformly mixing and stirring; adding thiosemicarbazide and formaldehyde, and uniformly mixing and stirring to obtain mixed monomer liquid;
A3, transferring the mixed monomer liquid into a hydrothermal kettle for solidification, cooling, respectively cleaning the mixed monomer liquid with deionized water and absolute ethyl alcohol, centrifuging to obtain a product, and drying the product in a vacuum drying oven at 60 ℃ for 24 hours to obtain the thiosemicarbazide modified composite resin;
A4, weighing Congo red with a certain mass, dissolving in deionized water, and dripping NaOH to adjust the pH value to 9 to obtain a Congo red solution; mixing the modified amino thiourea and the composite resin, and stirring until the solution is colorless; discarding clear liquid, adding Congo red solution, mixing and stirring until the color of the solution is no longer light; and washing off the floating color by deionized water and washing to neutrality to obtain the composite resin for adsorbing Congo red.
The synthesis reaction principle of the thiosemicarbazide modified composite resin is as follows:
In the reaction process of synthesizing phenolic resin by resorcinol and formaldehyde monomers, thiosemicarbazide is added for grafting modification; in addition, the melamine formaldehyde resin can also perform condensation reaction with formaldehyde, and the phenolic hydroxyl groups of the melamine formaldehyde resin and the resorcinol can perform amination reaction, so that the thiosemicarbazide modified composite resin is obtained through the reaction.
The synthetic reaction principle of the composite resin for adsorbing Congo red is as follows:
And complexing and adsorbing the congo red and the prepared thiosemicarbazide modified composite resin to obtain the congo red-adsorbed composite resin. The adsorption of the thiosemicarbazide modified composite resin and Congo red has double beneficial effects: on one hand, diversified functional groups for adsorbing Au and Ag can be further introduced; on the other hand, the molecular weight of the resin can be further increased, and the specificity of adsorption complexation is improved.
Further, resorcinol, melamine formaldehyde resin, thiosemicarbazide and formaldehyde are mixed according to a dosage ratio of 10g to 5g to 3 mL.
Further, the curing temperature is 100 ℃ and the curing time is 20 hours.
Further, the mixed solution and the congo red-adsorbed resin are mixed according to the dosage ratio of 200mL to 5g.
Further, the specific steps of the high-temperature roasting and deliquescing and secondary high-temperature roasting process of the ferric sulfate solid are as follows:
Adding the ferric sulfate solid into a muffle furnace, and roasting at a high temperature of 250 ℃ for 100-110min. Spraying 20mL of deionized water to the roasted ferric sulfate solid for deliquescence, wherein the deliquescence time is 24 hours; and adding 100mL of deionized water into the deliquesced material, standing, pouring out, and washing residues with water. Pouring the poured concentrated solution into a surface dish, and then placing the surface dish into a muffle furnace for secondary roasting, wherein the roasting temperature is 250-260 ℃ and the roasting time is 100min, and the obtained solid is anhydrous ferric sulfate.
And (3) carrying out an aging oxidation-high-temperature roasting-deliquescence-secondary high-temperature roasting process on pyrite cinder from which copper, gold and silver elements have been extracted, so as to prepare a final product, namely anhydrous ferric sulfate.
The invention has the following beneficial effects:
When the slag is used as refractory ore, firstly adopting an ammonia leaching method to extract copper element when nonferrous metals in the slag are extracted; then adopting designed specific resin to efficiently adsorb heavy metals such as gold and silver in the cinder; finally, the rest solid is roasted at high temperature to obtain anhydrous ferric sulfate;
The invention designs chelate resin with specific structure and functional group to chelate heavy metal gold and silver, and by grafting different functional groups, the chelate resin can form stronger acting force with different metal ions. The functional groups such as-NH-, -C=S-N-and the like contain N, S atoms, and can carry out coordination reaction with gold and silver metal ions to form a bond and a coordination bond with larger strength. In addition, the designed chelate resin has electrostatic field and space three-dimensional blocking effect, so that the selectivity of the chelate resin to specific metal ions is obviously higher than that of low-molecular organic reagents.
Detailed Description
The technical solutions of the present invention will be clearly and completely described in connection with the embodiments, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
S1, ammonia leaching of pyrite cinder
Weighing 30g of pyrite cinder, crushing to 50 meshes, adding the powder into a beaker, adding 100mL of 20 wt% ammonia water into the beaker, placing the beaker containing the ammonia water into an electric furnace for heating until the temperature in the beaker is 40 ℃, mixing and stirring for 30min at 100r/min, and then carrying out solid-liquid separation to obtain filtrate and filter residues; wherein the filtrate is the copper ammonium mixed solution.
S2, preparation of composite resin for adsorbing Congo red
100ML of deionized water and 20mL of 95%wt ethanol are added into a three-necked flask with the capacity of 500mL and mixed to obtain a solvent; then, regulating the pH value of the mixed solution to 7 by using 30 wt% NaOH solution to obtain the mixed solution; wherein the three-necked flask was equipped with a magnetic stirrer and a reflux condenser. And stirring the mixed solution at a constant speed of 30r/min for 60min at 30 ℃ to obtain mother solution.
Then adding 10g of resorcinol and 10g of melamine formaldehyde resin into the mother solution, and stirring at a constant speed of 30r/min for 30min; then adding 5g of thiosemicarbazide, and stirring at a constant speed of 30r/min for 1min; then adding 3mL of formaldehyde, and stirring at a constant speed of 30r/min for 200min to obtain mixed monomer liquid.
Transferring the mixed monomer liquid into a hydrothermal kettle, solidifying for 20 hours at 90 ℃, cooling, respectively cleaning the mixed monomer liquid with deionized water and absolute ethyl alcohol, centrifuging, separating the mixture to obtain a product, and drying the product in a vacuum drying oven at 60 ℃ for 24 hours to obtain the thiosemicarbazide modified composite resin.
Weighing 5g of Congo red powder, dissolving in water, and dripping NaOH to adjust the pH value to 9 to obtain a Congo red solution; mixing the modified amino thiourea and the composite resin, and stirring until the solution is colorless; removing clear liquid, adding Congo red solution, mixing and stirring until the color of the solution is not light, namely, the thiosemicarbazide modified composite resin adsorbs Congo red to be saturated, and then washing off the floating color by deionized water and flushing to be neutral to obtain the composite resin adsorbing Congo red.
S3, pyrite cinder resin adsorption
4ML of sulfuric acid of 20% wt and 200mL of deionized water were mixed to give an acidification system. Mixing the chlorination system and the filter residue according to a liquid-solid ratio of 3:1 at 55 ℃, dissolving the filter residue, and stirring at 400rpm for 20min to obtain a chlorinated mixed solution.
30ML of the chlorinated mixed solution and 5mg of resin for adsorbing Congo red are mixed, then the mixture is adsorbed for 12 hours in a 50mL brown volumetric flask, and the solid is filtered, namely the composite resin for adsorbing Au and Ag.
S4, preparing anhydrous ferric sulfate
Placing 100mL of filtrate in a porcelain bowl, adding 50mL of sulfuric acid with the weight of 20% and mixing and stirring at the speed of 100r/min to obtain a mixed solution; and heating the porcelain bowl until the mixed solution is fired into a solidified material block by liquid, and cooling to room temperature. And transferring the porcelain bowl into a fume hood, and standing for 24 hours at room temperature to obtain ferric sulfate solid.
The ferric sulfate solid is added into a muffle furnace and baked at a high temperature of 250 ℃ for 100min. Spraying 20mL of deionized water to the roasted ferric sulfate solid for deliquescence, wherein the deliquescence time is 24 hours; and adding 100mL of deionized water into the deliquesced material, standing, pouring out, and washing residues with water. Pouring the poured concentrated solution into a surface dish, and then putting the surface dish into a muffle furnace for secondary roasting, wherein the roasting temperature is 250 ℃ and the roasting time is 100min, and the obtained solid is anhydrous ferric sulfate.
Example 2
S1, ammonia leaching of pyrite cinder
Weighing 30g of pyrite cinder, crushing to 80 meshes, adding the crushed pyrite cinder into a beaker, adding 120mL of 20%wt ammonia water into the beaker, placing the beaker containing the ammonia water into an electric furnace for heating until the temperature in the beaker is 44 ℃, mixing and stirring for 30min at 100r/min, and then carrying out solid-liquid separation to obtain filtrate and filter residues; wherein the filtrate is the copper ammonium mixed solution.
According to the method, ammonia water is adopted to leach the pyrite cinder in advance, copper and ammonia molecules can form copper ammonia complex, copper can be leached out, iron is remained in the cinder because of being insoluble in the ammonia water, so that a large amount of iron contained in the cinder cannot be lost, and effective separation of copper is realized. In addition, in the ammonia leaching process, the gold and silver which are heavy metal elements to be recovered are not reacted with ammonia water due to low activity, so that the heavy metal elements are reserved in pyrite cinder.
S2, preparation of composite resin for adsorbing Congo red
100ML of deionized water and 20mL of 95%wt ethanol are added into a three-necked flask with the capacity of 500mL and mixed to obtain a solvent; then, regulating the pH value of the mixed solution to 7-8 by using 30 wt% NaOH solution to obtain the mixed solution; wherein the three-necked flask was equipped with a magnetic stirrer and a reflux condenser. And stirring the mixed solution at a constant speed of 35r/min for 60min at 30 ℃ to obtain mother solution.
Then adding 10g of resorcinol and 10g of melamine formaldehyde resin into the mother solution, and stirring at a constant speed of 40r/min for 30min; then adding 5g of thiosemicarbazide, and stirring at a constant speed of 35r/min for 1min; then 4mL of formaldehyde is added, and the mixture is stirred at a constant speed of 45r/min for 200min, so as to obtain mixed monomer liquid.
Transferring the mixed monomer liquid into a hydrothermal kettle, solidifying for 20 hours at 95 ℃, cooling, respectively cleaning the mixed monomer liquid with deionized water and absolute ethyl alcohol, centrifuging, separating the mixture to obtain a product, and drying the product in a vacuum drying oven at 60 ℃ for 24 hours to obtain the thiosemicarbazide modified composite resin.
8G of Congo red powder is weighed and dissolved in water, and NaOH is added dropwise to adjust the pH value to 9, so as to obtain a Congo red solution; mixing the modified amino thiourea and the composite resin, and stirring until the solution is colorless; removing clear liquid, adding Congo red solution, mixing and stirring until the color of the solution is not light, namely, the thiosemicarbazide modified composite resin adsorbs Congo red to be saturated, and then washing off the floating color by deionized water and flushing to be neutral to obtain the composite resin adsorbing Congo red.
S3, pyrite cinder resin adsorption
4ML of sulfuric acid of 20% wt and 200mL of deionized water were mixed to give an acidification system. Mixing the chlorination system and the filter residue according to a liquid-solid ratio of 3:1 at 55 ℃, dissolving the filter residue, and stirring for 20min at 405rpm to obtain a chlorinated mixed solution.
30ML of the chlorinated mixed solution and 5mg of resin for adsorbing Congo red are mixed, then the mixture is adsorbed for 12 hours in a 50mL brown volumetric flask, and the solid is filtered, namely the composite resin for adsorbing Au and Ag.
S4, preparing anhydrous ferric sulfate
Placing 100mL of filtrate in a porcelain bowl, adding 50mL of sulfuric acid with the weight of 20% and mixing and stirring at 110r/min to obtain a mixed solution; and heating the porcelain bowl until the mixed solution is fired into a solidified material block by liquid, and cooling to room temperature. And transferring the porcelain bowl into a fume hood, and standing for 24 hours at room temperature to obtain ferric sulfate solid.
The ferric sulfate solid is added into a muffle furnace and baked for 120min at a high temperature of 250 ℃. Spraying 25mL of deionized water to the roasted ferric sulfate solid for deliquescence, wherein the deliquescence time is 24 hours; and adding 100mL of deionized water into the deliquesced material, standing, pouring out, and washing residues with water. Pouring the poured concentrated solution into a surface dish, and then putting the surface dish into a muffle furnace for secondary roasting, wherein the roasting temperature is 250 ℃ and the roasting time is 110min, and the obtained solid is anhydrous ferric sulfate.
Example 3
S1, ammonia leaching of pyrite cinder
Weighing 30g of pyrite cinder, crushing to 100 meshes, adding the 100 meshes into a beaker, adding 150mL of 20%wt ammonia water into the beaker, placing the beaker containing the ammonia water into an electric furnace for heating until the temperature in the beaker is 50 ℃, mixing and stirring for 30min at 100r/min, and then carrying out solid-liquid separation to obtain filtrate and filter residues; wherein the filtrate is the copper ammonium mixed solution.
According to the method, ammonia water is adopted to leach the pyrite cinder in advance, copper and ammonia molecules can form copper ammonia complex, copper can be leached out, iron is remained in the cinder because of being insoluble in the ammonia water, so that a large amount of iron contained in the cinder cannot be lost, and effective separation of copper is realized. In addition, in the ammonia leaching process, the gold and silver which are heavy metal elements to be recovered are not reacted with ammonia water due to low activity, so that the heavy metal elements are reserved in pyrite cinder.
S2, preparation of composite resin for adsorbing Congo red
100ML of deionized water and 20mL of 95%wt ethanol are added into a three-necked flask with the capacity of 500mL and mixed to obtain a solvent; then, regulating the pH value of the mixed solution to 7-8 by using 30 wt% NaOH solution to obtain the mixed solution; wherein the three-necked flask was equipped with a magnetic stirrer and a reflux condenser. And stirring the mixed solution at a constant speed of 50r/min for 60min at 30 ℃ to obtain mother solution.
Then adding 10g of resorcinol and 10g of melamine formaldehyde resin into the mother solution, and stirring at a constant speed of 50r/min for 30min; then adding 5g of thiosemicarbazide, and stirring at a constant speed of 50r/min for 1min; then 5mL of formaldehyde is added, and the mixture is stirred at a constant speed of 0r/min for 200min, so as to obtain mixed monomer liquid.
Transferring the mixed monomer liquid into a hydrothermal kettle, solidifying for 20 hours at the temperature of 100 ℃, cooling, respectively cleaning the mixed monomer liquid with deionized water and absolute ethyl alcohol, centrifuging, separating the mixture to obtain a product, and drying the product in a vacuum drying oven at the temperature of 60 ℃ for 24 hours to obtain the thiosemicarbazide modified composite resin.
Weighing 10g of Congo red powder, dissolving in water, and dripping NaOH to adjust the pH value to 9 to obtain a Congo red solution; mixing the modified amino thiourea and the composite resin, and stirring until the solution is colorless; removing clear liquid, adding Congo red solution, mixing and stirring until the color of the solution is not light, namely, the thiosemicarbazide modified composite resin adsorbs Congo red to be saturated, and then washing off the floating color by deionized water and flushing to be neutral to obtain the composite resin adsorbing Congo red.
S3, pyrite cinder resin adsorption
4ML of sulfuric acid of 20% wt and 200mL of deionized water were mixed to give an acidification system. Mixing the chlorination system and the filter residue according to a liquid-solid ratio of 3:1 at 55 ℃, dissolving the filter residue, and stirring at 400rpm for 20min to obtain a chlorinated mixed solution.
30ML of the chlorinated mixed solution and 5mg of resin for adsorbing Congo red are mixed, then the mixture is adsorbed for 12 hours in a 50mL brown volumetric flask, and the solid is filtered, namely the composite resin for adsorbing Au and Ag.
S4, preparing anhydrous ferric sulfate
Placing 100mL of filtrate in a porcelain bowl, adding 50mL of sulfuric acid with the weight of 20% and mixing and stirring at the speed of 100r/min to obtain a mixed solution; and heating the porcelain bowl until the mixed solution is fired into a solidified material block by liquid, and cooling to room temperature. And transferring the porcelain bowl into a fume hood, and standing for 24 hours at room temperature to obtain ferric sulfate solid.
The ferric sulfate solid is added into a muffle furnace and baked at a high temperature of 250 ℃ for 110min. Spraying 20mL of deionized water to the roasted ferric sulfate solid for deliquescence, wherein the deliquescence time is 24 hours; and adding 100mL of deionized water into the deliquesced material, standing, pouring out, and washing residues with water. Pouring the poured concentrated solution into a surface dish, and then putting the surface dish into a muffle furnace for secondary roasting, wherein the roasting temperature is 260 ℃ and the roasting time is 100min, and the obtained solid is anhydrous ferric sulfate.
The foregoing is merely illustrative and explanatory of the invention, as it is well within the scope of the invention as claimed, as it relates to various modifications, additions and substitutions for those skilled in the art, without departing from the inventive concept and without departing from the scope of the invention as defined in the accompanying claims.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended only to assist in the explanation of the invention. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise form disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best understand and utilize the invention. The invention is limited only by the claims and the full scope and equivalents thereof.
Claims (7)
1. The method for preparing anhydrous ferric phosphate by using pyrite reduction roasting is characterized by comprising the following steps:
S1, weighing a certain amount of pyrite cinder, crushing to 50-100 meshes, and mixing with ammonia water to obtain a mixture; heating the mixture until the heating temperature of the mixture reaches 40-50 ℃, mixing and stirring to react for 30min, and then carrying out solid-liquid separation, wherein filtrate is copper ammonia mixed solution; the filter residue is processed in the next step;
s2, mixing sulfuric acid with the weight of 20% with deionized water to obtain an acidification system; mixing an acidification system and filter residues according to a solid-to-liquid ratio of 1:3, and dissolving the filter residues to obtain a mixed solution;
s3, mixing the mixed solution with the resin for adsorbing Congo red, adsorbing for 12 hours, and filtering the solid, wherein the solid is the composite resin for adsorbing Au and Ag; the filtrate is processed in the next step;
s4, mixing the filtrate with sulfuric acid to obtain a mixed solution; heating the porcelain bowl until the mixed solution is fired into a solidified material block by liquid, and cooling to room temperature; transferring the porcelain bowl into a fume hood, and standing for 24 hours at room temperature to obtain ferric sulfate solid;
s5, performing high-temperature roasting, deliquescing and secondary high-temperature roasting on the ferric sulfate solid to obtain the purified ferric sulfate solid.
2. The method for preparing anhydrous ferric phosphate by reductive roasting of pyrite according to claim 1, wherein the mixing amount ratio of pyrite cinder and ammonia water is 30g:100-150mL, and the concentration of ammonia water is 20%wt.
3. The method for preparing anhydrous ferric phosphate by using pyrite reduction roasting according to claim 1, wherein the resin preparation method for adsorbing congo red in S3 specifically comprises the following steps:
A1, mixing 100mL of deionized water with 5%wt of 20mL of ethanol to obtain a solvent; then, regulating the pH value of the solvent to 7-8 by using 30 wt% NaOH solution to obtain a mixed solution; stirring the mixed solution at a constant speed of 30-50r/min for 60min to obtain mother solution;
a2, adding resorcinol and melamine formaldehyde resin into the mother liquor, and uniformly mixing and stirring; adding thiosemicarbazide and formaldehyde, and uniformly mixing and stirring to obtain mixed monomer liquid;
A3, transferring the mixed monomer liquid into a hydrothermal kettle for solidification, cooling, respectively cleaning the mixed monomer liquid with deionized water and absolute ethyl alcohol, centrifuging to obtain a product, and drying the product in a vacuum drying oven at 60 ℃ for 24 hours to obtain the thiosemicarbazide modified composite resin;
A4, weighing Congo red with a certain mass, dissolving in deionized water, and dripping NaOH to adjust the pH value to 9 to obtain a Congo red solution; mixing the modified amino thiourea and the composite resin, and stirring until the solution is colorless; discarding clear liquid, adding Congo red solution, mixing and stirring until the color of the solution is no longer light; and washing off the floating color by deionized water and washing to neutrality to obtain the composite resin for adsorbing Congo red.
4. The method for preparing anhydrous ferric phosphate by using pyrite reduction roasting according to claim 3, wherein the resorcinol, melamine formaldehyde resin, thiosemicarbazide and formaldehyde are mixed according to the dosage ratio of 10g to 5g:3-5 mL.
5. The method for preparing anhydrous ferric phosphate by reductive roasting of pyrite according to claim 3, wherein the solidification temperature is 90-100 ℃ and the solidification time is 20h.
6. The method for preparing anhydrous ferric phosphate by reductive roasting of pyrite according to claim 3, wherein the mixed solution and the resin adsorbing congo red are mixed according to the dosage ratio of 200ml:5-10 g.
7. The method for preparing anhydrous ferric phosphate by using pyrite reduction roasting according to claim 1, wherein the specific steps of the high-temperature roasting, deliquescing and secondary high-temperature roasting process of the ferric sulfate solid are as follows:
Adding ferric sulfate solid into a muffle furnace, and roasting at a high temperature of 250 ℃ for 100-110min; spraying 20mL of deionized water to the roasted ferric sulfate solid for deliquescence, wherein the deliquescence time is 24 hours; adding 100mL of deionized water into the deliquesced material, standing, pouring out, and washing residues with water; pouring the poured concentrated solution into a surface dish, and then placing the surface dish into a muffle furnace for secondary roasting, wherein the roasting temperature is 250-260 ℃ and the roasting time is 100min, and the obtained solid is anhydrous ferric sulfate.
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| CN202410359681.4A Pending CN118145713A (en) | 2024-03-27 | 2024-03-27 | Method for preparing anhydrous ferric phosphate by reduction roasting of pyrite |
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