CN1958462A - Method for preparing potassium ferrate by using waste liquid from acid washing steel - Google Patents
Method for preparing potassium ferrate by using waste liquid from acid washing steel Download PDFInfo
- Publication number
- CN1958462A CN1958462A CN 200610124990 CN200610124990A CN1958462A CN 1958462 A CN1958462 A CN 1958462A CN 200610124990 CN200610124990 CN 200610124990 CN 200610124990 A CN200610124990 A CN 200610124990A CN 1958462 A CN1958462 A CN 1958462A
- Authority
- CN
- China
- Prior art keywords
- filtrate
- solution
- potassium ferrate
- waste liquid
- kclo
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Compounds Of Iron (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
This invention relates to a method preparing potassium ferrate from steel acid-washing waste liquid. The method comprises: oxidizing bivalent iron ions in steel acid-washing waste liquid into trivalent iron ions, precipitating trivalent iron ions to obtain Fe (OH) 3, and oxidizing Fe (OH) 3 by KClO in a strong alkaline condition to obtain potassium ferrate. The process mainly comprises: catalytically oxidizing, filtering the precipitate, oxidizing by KClO, recovering the filtrate, recrystallizing for purification, and washing with organic solvent. The method is environmentally friendly.
Description
Technical Field
The invention belongs to the field of resource utilization of steel pickling waste liquid, and particularly relates to a method for preparing potassium ferrate by using the steel pickling waste liquid.
Background
In the processing of steel products, the surfaces of the steel products are often subjected to pickling rust removal treatment by hydrochloric acid or sulfuric acid, thereby generating a large amount of pickling waste liquid. At present, the treatment methods of the waste acid mainly comprise a neutralization method, a high-temperature roasting method, electrodialysis, an ion exchange membrane, nanofiltration and the like, and the methods have the problems of secondary pollution, high treatment cost and low social and economic benefits or can not completely recycle and utilize the acid and the iron.
Ferric (fe (vi)) chloride salt is a stronger oxidizing agent than potassium permanganate and chlorine. The potassium ferrate product with higher purity is black and glossy powdery crystal, has a melting point of 198 ℃, is very easy to dissolve in water to generate a mauve solution, and has strong oxidizing property in the whole pH range.
Ferrate is gaining increasing attention from water treatment researchers due to its dual efficacy of strong oxidative sterilization and flocculation purification. As is well known, flocculation purification and oxidation sterilization are two important unit operations in water treatment, which are used to remove colloidal particles and harmful substances from water, traditional flocculants are ferric sulfate (or chloride), aluminum salt, etc., while oxidation sterilization is mainly chlorine gas, sodium hypochlorite, chlorine dioxide, etc. With the aggravation of water pollution problem and the improvement of drinking water standard, especially the discovery that free chlorine can react with organic matters in water to generate trichloromethane and other chlorinated hydrocarbon carcinogenic substances, a safe, efficient and even multi-effect water treatment agent is urgently needed to be developed. Ferrate is reduced by its strong oxidizing and water reducing products Fe (OH)3The flocculation of (2) can meet the above requirements, and free Fe3+、Fe2+It also has effects of supplementing iron and replenishing blood. Therefore, the ferrate is a safe and double-effect water treatment flocculant integrating oxidation sterilization, flocculation decontamination. Meanwhile, the ferrate battery has a wide application prospect in the fields of industry, people, military and the like due to the superior characteristics of high energy, rechargeability and the like.
The known methods for producing ferrate include: 1. in the dry method, which is a high-temperature solid-phase reaction method, under the condition of caustic alkali, oxidants such as potassium nitrate or peroxide can oxidize iron salt or iron oxide into ferrate at high temperature. 2. In the wet method, hypochlorite and ferric salt are used as raw materials, and the hypochlorite fully oxidizes ferric iron in an alkaline solution to generate ferrate. 3. Electrolysis, electrolysis in concentrated alkaline solution at a suitable current density, iron dissolution at the anode and ferrate generation. Wherein, the wet process is the most mature, the investment equipment is less, the ferrate with higher purity can be prepared, and the method is the most studied one in the prior preparation methods. However, in the operation process of purification and separation, a large amount of potassium hydroxide is added, and a large amount of waste alkali liquor is generated after filtration, so that not only is resources greatly wasted, but also the environment is seriously polluted.
Disclosure of Invention
The invention aims to provide a method for preparing potassium ferrate by using steel pickling waste liquid, which is environment-friendly and low in cost.
In order to achieve the purpose, the technical scheme of the invention is as follows: a method for preparing potassium ferrate by using steel pickling waste liquid is characterized by comprising the following steps:
1) mixing the steel pickling waste liquid with hydrochloric acid with the mass fraction of 1-21% in a volume ratio of 1000: 6-40, aerating the mixed liquid by using an aerator, and heating to 40-90 ℃; when the temperature reaches 40-90 ℃, NaNO with the weight concentration of 1-50 per mill is added21-50% by weight of NaNO2The adding amount of the mixed solution is 0.1-5% of the mass of the mixed solution, continuously aerating, and reacting for 1-6 h under the condition of maintaining the temperature of the system at 40-90 ℃;
after the reaction is finished, adding the reaction solution into an alkali solution to obtain Fe3+With Fe (OH)3Is precipitated in the form of (1), wherein, OH-The total amount of the substances of (A) is Fe3+4 to 50 times of (1), and precipitating Fe (OH)3Filtering and washing for later use;
2) stirring the precipitate Fe (OH) of step 1)3Adding the KClO into a KClO concentrated alkali solution in 10-30 batches, wherein the KClO concentration in the KClO concentrated alkali solution is 1.2-2.8 mol/l, the alkali concentration is 10-20 mol/l, and the KClO and a precipitate Fe (OH)3The ratio of the amount of the substances is 1-4; the reaction is exothermic, ice water bath is used for controlling the temperature to be 0-50 ℃, and the mixture is fully stirred;
adding the precipitate Fe (OH) in 10-30 batches3The time is 0.5-4 hours, and then the reaction is continued for 10-60 min; adding KOH solid into the solution, wherein the mass ratio of the added KOH solid to the volume of the solution is 40:100-90: 100(g/ml), so that potassium ferrate is precipitated, and the temperature of the system is 10-30 ℃; relay (S)Continuously stirring for 1-30 minutes, cooling the system to below 0 ℃ in an ice-water bath, and quickly performing vacuum filtration by using a G1 glass sand core funnel to obtain a crude product and a filtrate A; recovering the filtrate A, and reusing the filtrate A in the alkali solution in the step 1);
3) purification and washing of the crude product: washing the crude product obtained in the step 2) with 0.1-6 mol/L KOH solution for 4-10 times to dissolve potassium ferrate, performing vacuum filtration by using a G2 glass sand core funnel to obtain a filtrate B, collecting the filtrate B, and performing vacuum filtration by using a G4 glass sand core funnel to obtain a filtrate C; then adding the filtrate C into a KOH solution with the temperature of 0 ℃ and the mol/L of 14, wherein the volume ratio of the filtrate C to the KOH solution is 1: 3-1: 5, and stirring for 5-30 minutes to separate out potassium ferrate crystals; quickly vacuum filtering the mixture by using a G3 glass sand core funnel to obtain K2FeO4Crystals and filtrate D; recovering the filtrate D, and recycling the filtrate D for the alkali solution in the step 1); then K is put2FeO4Leaching the crystal by using normal hexane, pentane and methanol respectively for four times in sequence, and leaching by using diethyl ether for two times;
4) and (3) drying: k after impurity removal2FeO4Vacuum drying the crystal at 60 deg.c for 12 hr to obtain potassium ferrate crystal with quality purity of 80-95.5%.
The iron and steel pickling waste liquid in the step 1) contains Fe2+0.1-20% by mass of Fe3+0.1-20% by mass of Cl-The mass percentage of the acid is 0.1-35%, and the acidity is 0-6 mol/l.
The alkali solution in the step 1) is a NaOH solution or a KOH solution, and the concentration of the alkali solution is 1-20 mol/L.
The invention firstly oxidizes a large amount of ferrous ions in the steel pickling waste liquid into ferric iron, and then the ferric iron is precipitated to obtain Fe (OH)3Then adding potassium hypochlorite to the Fe (OH) solution under the condition of strong alkalinity3The oxidation to ferrate comprises the following main processes: catalytic oxidation, precipitation filtration, hypochlorous acid oxidation, filtrate recycling, recrystallization purification, organic agent washing and the like. Well-known iron-source FeCl for preparing potassium ferrate3、Fe(NO3)3And the like. In wet processes, a solid iron source is generally used. In the present invention, a binding acid is usedThe washing waste liquid and the process for preparing potassium ferrate have the characteristics of no FeCl obtained after oxidation3Solution evaporation crystallization to prepare FeCl3Solid but FeCl3Mixing the solution with alkali liquor to obtain Fe (OH)3Precipitating, then Fe (OH)3The potassium hypochlorite is oxidized into the ferrate under the strong alkaline condition, so that the cost of an iron source is reduced, waste alkali liquor generated in the process of preparing the potassium ferrate is effectively recycled, waste is changed into valuable, and the method has good environmental benefit and economic benefit.
The preparation method has the advantages of continuous operation, less waste alkali liquor, low cost, and particularly, the waste alkali liquor generated in the production process can be recycled, so that the cost is greatly reduced; the steel pickling waste liquid is recycled, the environment pollution is prevented, and the invention has the environmental protection function.
The invention not only eliminates the pollution of the steel pickling waste liquid to the environment, but also widens the application field of the steel pickling waste liquid in the aspect of resource utilization. The potassium ferrate product obtained by the preparation method is a novel high-efficiency multifunctional water treatment agent integrating oxidation, adsorption, flocculation, coagulation aiding, sterilization and deodorization, and has a wide application range in the field of environmental protection. Meanwhile, the ferrate battery has a wide application prospect in the fields of industry, civil, military and the like due to the superior characteristics of high energy, rechargeability and the like.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
In order to better understand the present invention, the following examples are further provided to illustrate the present invention, but the present invention is not limited to the following examples.
Example 1:
a method for preparing potassium ferrate by using steel pickling waste liquid comprises the following steps:
1) mixing iron and steel acidWashing waste liquid (containing Fe)2+0.1% by mass of (B) and Fe3+Is 0.1% by mass, Cl-0.1% by mass, 0mol/l acidity) and 21% by mass of hydrochloric acid are mixed in a volume ratio of 1000: 6, the mixed solution is aerated by an aerator and heated to 40 ℃; when the temperature reaches 40 ℃, NaNO with the weight concentration of 1 per mill is added2NaNO with a weight concentration of 1 ‰2The adding amount of the mixed solution is 0.1 percent of the mass of the mixed solution, the aeration is continued, and the system is maintained to react for 1 hour at the temperature of 40 ℃; the reaction equation involved:
after the reaction is finished, adding the reaction solution into an alkali solution to obtain Fe3+With Fe (OH)3Is precipitated in the form of (1), wherein, OH-The total amount of the substances of (A) is Fe3+4 times of (1), and precipitating Fe (OH)3Filtering and washing for later use; the alkali solution is NaOH solution or KOH solution, and the concentration of the alkali solution is 1 mol/L;
2) under the condition of vigorous stirring (80-300 rpm), the precipitate Fe (OH) of the step 1) is mixed3Adding into concentrated alkali solution of KClO (KClO concentration is 1.2mol/l, alkali concentration is 10mol/l) in 10 batches, KClO and Fe (OH)3The ratio of the amounts of substances of (a) to (b) is 1; the reaction is exothermic, the temperature is controlled at 0 ℃ by using an ice water bath, and the mixture is fully stirred; the oxidation reaction is carried out quickly, and the color of the solution is immediately changed into purple black; the reaction equation involved is:
the precipitate Fe (OH) is added in 10 portions3For 0.5 hour, and then continuing the reaction for 10 min; adding KOH solid into the solution, wherein the mass ratio of the added KOH solid to the volume of the solution is 40: 100(g/ml), so that potassium ferrate is precipitated, and the temperature of the system is 10 ℃; stirring for 1min, cooling to below 0 deg.C (-1 deg.C) with ice water bath, and quickly vacuum-pumping with G1 glass sand core funnelCarrying out suction filtration to obtain a crude product and a filtrate A; recovering the filtrate A, and reusing the filtrate A in the alkali solution in the step 1);
3) purification and washing of the crude product: washing the crude product obtained in the step 2) with 0.1mol/L KOH solution for 4 times to dissolve potassium ferrate, filtering with G2 to obtain filtrate B, collecting the filtrate B, vacuum-filtering with a G4 glass sand core funnel,obtaining filtrate C; then adding the filtrate C into a KOH solution with the temperature of 0 ℃ and the mol/L of 14, wherein the volume ratio of the filtrate C to the KOH solution is 1: 3, and stirring for 5 minutes to separate out potassium ferrate crystals; quickly vacuum filtering the mixture by using a G3 glass sand core funnel to obtain K2FeO4Crystals and filtrate D; recovering the filtrate D, and recycling the filtrate D for the alkali solution in the step 1); then K is put2FeO4The crystal is leached by n-hexane, pentane and methanol respectively for four times and by diethyl ether for two times in sequence to remove residual H in the product2O, KOH and KCl;
4) and (3) drying: k after impurity removal2FeO4Vacuum drying the crystal at 60 deg.c for 12 hr to obtain potassium ferrate crystal with quality purity of 80-95.5%. Weighing, and storing in a vacuum drier with silica gel water absorbent.
Example 2:
a method for preparing potassium ferrate by using steel pickling waste liquid comprises the following steps:
1) pickling waste liquid (containing Fe) of steel2+Is 10% by mass, Fe3+Is 10% by mass, Cl-20 percent of acid, 3mol/l) and hydrochloric acid with the mass fraction of 10 percent are mixed according to the volume ratio of 1000: 30, the mixed solution is aerated by an aerator and is heated to 70 ℃; when the temperature reaches 70 ℃, NaNO with the weight concentration of 30 per mill is added2NaNO with weight concentration of 30 per mill2The adding amount of the mixed solution is 2 percent of the mass of the mixed solution, the aeration is continued, and the system is maintained to react for 4 hours at the temperature of 70 ℃; the reaction equation involved:
after the reaction is finished, adding the reaction solution into an alkali solution to obtain Fe3+With Fe (OH)3Is precipitated in the form of (1), wherein, OH-The total amount of the substances of (A) is Fe3+30 times of the above, and the precipitate Fe (OH)3Filtering and washing for later use; the alkali solution is NaOH solution or KOH solution, and the concentration of the alkali solution is 10 mol/L;
2) under the condition of vigorous stirring (80-300 rpm), the precipitate Fe (OH) of the step 1) is mixed3Adding into concentrated alkali solution of KClO (KClO concentration is 2.0mol/l, alkali concentration is 15mol/l) in 20 batches, KClO and Fe (OH)3The ratio of the amounts of substances of (a) to (b) is 3; the reaction is exothermic, the temperature is controlled at 30 ℃ by using ice water bath, and the mixture is fully stirred; the oxidation reaction is carried out quickly, and the color of the solution is immediately changed into purple black; the reaction equation involved is:
the precipitate Fe (OH) is added in 20 portions3The reaction time is 3 hours, and then the reaction is continued for 30 min; adding KOH solid into the solution, wherein the mass ratio of the added KOH solid to the volume of the solution is 60: 100(g/ml), so that the potassium ferrate is precipitated, and the temperature of the system is 20 ℃; continuously stirring for 20 minutes, cooling the system to below 0 ℃ (0.5 ℃) by ice-water bath, and quickly performing vacuum filtration by using a G1 glass sand core funnel to obtain a crude product and a filtrate A; recovering the filtrate A, and reusing the filtrate A in the alkali solution in the step 1);
3) purification and washing of the crude product: washing the crude product obtained in the step 2) with 3mol/L KOH solution for 7 times to dissolve potassium ferrate, filtering with G2 to obtain filtrate B, collecting the filtrate B, and performing vacuum filtration with a G4 glass sand core funnel to obtain filtrate C; then adding the filtrate C into a KOH solution with the temperature of 0 ℃ and the mol/L of 14, wherein the volume ratio of the filtrate C to the KOH solution is 1: 4, and stirring for 20 minutes to separate out potassium ferrate crystals; quickly vacuum filtering the mixture by using a G3 glass sand core funnel to obtain K2FeO4Crystals and filtrate D; recovering the filtrate D, and recycling the filtrate D for the alkali solution in the step 1); then K is put2FeO4The crystal is leached by n-hexane, pentane and methanol respectively for four times and by diethyl ether for two times in sequence to remove residual H in the product2O、KOHAnd KCl and the like;
4) and (3) drying: k after impurity removal2FeO4Vacuum drying the crystal at 60 deg.c for 12 hr to obtain potassium ferrate crystal with quality purity of 80-95.5%. Weighing, and storing in a vacuum drier with silica gel water absorbent.
Example 3:
a method for preparing potassium ferrate by using steel pickling waste liquid comprises the following steps:
1) pickling waste liquid (containing Fe) of steel2+20% by mass of (C) Fe3+20% by mass of (C), Cl-35 percent of acid, 6mol/l) and 21 percent of hydrochloric acid in a volume ratio of 1000: 40, aerating the mixed solution by an aerator, and heating to 90 ℃; when the temperature reaches 90 ℃, NaNO with the weight concentration of 50 per mill is added2NaNO with 50 per mill of weight concentration2The adding amount of the mixed solution is 5 percent of the mass of the mixed solution, the aeration is continued, and the system is maintained to react for 6 hours at the temperature of 90 ℃; the reaction equation involved:
after the reaction is finished, adding the reaction solution into an alkali solution to obtain Fe3+With Fe (OH)3Is precipitated in the form of (1), wherein, OH-The total amount of the substances of (A) is Fe3+50 times of the above, and the precipitate Fe (OH)3Filtering and washing for later use; the alkali solution is NaOH solution or KOH solution, and the concentration of the alkali solution is 20 mol/L;
2) under the condition of vigorous stirring (80-300 rpm), the precipitate Fe (OH) of the step 1) is mixed3Adding into concentrated alkali solution of KClO (KClO concentration is 2.8mol/l, alkali concentration is 20mol/l) in 30 batches, KClO and Fe (OH)3The ratio of the amounts of substances of (a) to (b) is 4; the reaction is exothermicControlling the temperature at 50 ℃ by using an ice water bath, and fully stirring; the oxidation reaction is carried out quickly, and the color of the solution is immediately changed into purple black; the reaction equation involved is:
the precipitate Fe (OH) is added in 30 portions3For 4 hours, and then continuing the reaction for 60 min; adding KOH solid into the solution, wherein the mass ratio of the added KOH solid to the volume of the solution is 90: 100(g/ml), so that potassium ferrate is precipitated, and the temperature of the system is 30 ℃; continuously stirring for 30 minutes, cooling the system to below 0 ℃ (1.5 ℃) by ice-water bath, and quickly performing vacuum filtration by using a G1 glass sand core funnel to obtain a crude product and a filtrate A; recovering the filtrate A, and reusing the filtrate A in the alkali solution in the step 1);
3) purification and washing of the crude product: washing the crude product obtained in the step 2) with 6mol/L KOH solution for 10 times to dissolve potassium ferrate, filtering with G2 to obtain filtrate B, collecting the filtrate B, and performing vacuum filtration with a G4 glass sand core funnel to obtain filtrate C; then adding the filtrate C into a KOH solution with the temperature of 0 ℃ and the mol/L of 14, wherein the volume ratio of the filtrate C to the KOH solution is 1: 5, and stirring for 30 minutes to separate out potassium ferrate crystals; quickly vacuum filtering the mixture by using a G3 glass sand core funnel to obtain K2FeO4Crystals and filtrate D; recovering the filtrate D, and recycling the filtrate D for the alkali solution in the step 1); then K is put2FeO4The crystal is leached by n-hexane, pentane and methanol respectively for four times and by diethyl ether for two times in sequence to remove residual H in the product2O, KOH and KCl;
4) and (3) drying: k after impurity removal2FeO4Vacuum drying the crystal at 60 deg.c for 12 hr to obtain potassium ferrate crystal with quality purity of 80-95.5%. Weighing, and storing in a vacuum drier with silica gel water absorbent.
Examples of the use of the prepared potassium ferrate are:
for landfill leachate, the biological method is the most common method, and the specific processes are an activated sludge method, a stabilization pond, a biological rotating disk, an anaerobic fixed membrane bioreactor and the like. The treatment of landfill leachate by a biological method is generally not thorough, COD and ammonia nitrogen are still high after the treatment, and the discharge standard is difficult to reach, so that the landfill leachate also needs to be subjected to advanced treatment. When aluminum salt or ferric salt is used as a flocculating agent for deeply treating the landfill leachate, the removal rate of COD can reach 50 percent, but the method can generate a large amount of sludge and has low removal rate of ammonia nitrogen. When the potassium ferrate is used for the advanced treatment of the landfill leachate, the maximum removal rates of COD and ammonia nitrogen respectively reach 80 percent and 75 percent. The result shows that the potassium ferrate has better treatment effect on the landfill leachate as a high-efficiency multifunctional water treatment agent.
The potassium ferrate as a high-efficiency bactericide has wide application in water treatment. The natural water without serious pollution can be filtered by river sand or clarified by alum, and then proper amount of K is added2FeO4And (5) sterilizing the powder. According to the different pollution degree of water source (such as river water, lakewater, well water and rainwater), different dosage is used, generally when K is equal to K2FeO4When the concentration of the water sample is 5-6 mg/L, the sterilization efficiency reaches 99.95% -99.99%, and meanwhile, the chroma and turbidity are also obviously reduced. K2FeO4Have been used for the ambient disinfection of temporary water for sexual life by field workers.
Ferrate is reduced to form ferric salt or ferric hydroxide after oxidizing organic matter and microbes in water. Ferric hydroxide is a flocculant with excellent performance. The turbidity of the water treated with ferrate, ferrous sulfate heptahydrate, and ferric nitrate was compared. The results show that: the turbidity of the residue in the waste water treated with ferrate is less than that of the residue treated with ferrous sulfate and ferric nitrate. Another advantage of using ferrate is that: it can destabilize colloid particles within 1min, while ferrous sulfate and ferric nitrate can achieve the same removal effect only after being mixed for 30 min.
Ferrate is a novel high-efficiency multifunctional water treatment agent integrating oxidation, adsorption, flocculation, coagulation aid, sterilization and deodorization. It attracts more and more scholars to research and develop the preparation process and application with the unique water treatment function. With the continuous optimization of the preparation process of the potassium ferrate, the purity and the yield of the product are gradually improved, the application field of the potassium ferrate is gradually widened, and the demand of the product tends to increase year by year in the international market.
Claims (3)
1. A method for preparing potassium ferrate by using steel pickling waste liquid is characterized by comprising the following steps:
1) mixing the steel pickling waste liquid with hydrochloric acid with the mass fraction of 1-21% in a volume ratio of 1000: 6-40, aerating the mixed liquid by using an aerator, and heating to 40-90 ℃; when the temperature reaches 40-90 ℃, NaNO with the weight concentration of 1-50 per mill is added21-50% by weight of NaNO2The adding amount of the mixed solution is 0.1-5% of the mass of the mixed solution, continuously aerating, and reacting for 1-6 h under the condition of maintaining the temperature of the system at 40-90 ℃;
after the reaction is finished, adding the reaction solution into an alkali solution to obtain Fe3+With Fe (OH)3Is precipitated in the form of (1), wherein, OH-The total amount of the substances of (A) is Fe3+4 to 50 times of (1), and precipitating Fe (OH)3Filtering and washing for later use;
2) stirring the precipitate Fe (OH) of step 1)3Adding the KClO into a KClO concentrated alkali solution in 10-30 batches, wherein the KClO concentration in the KClO concentrated alkali solution is 1.2-2.8 mol/l, the alkali concentration is 10-20 mol/l, and the KClO and a precipitate Fe (OH)3The ratio of the amount of the substances is 1-4; the reaction is exothermic, ice water bath is used for controlling the temperature to be 0-50 ℃, and the mixture is fully stirred;
adding the precipitate Fe (OH) in 10-30 batches3The time is 0.5-4 hours, and then the reaction is continued for 10-60 min; adding KOH solid into the solution, wherein the mass ratio of the added KOH solid to the volume of the solution is 40: 100-90: 100(g/ml), so that potassium ferrate is precipitated, and the temperature of the system is 10-30 ℃; continuously stirring for 1-30 minutes, cooling the system to below 0 ℃ in an ice-water bath, and quickly performing vacuum filtrationby using a G1 glass sand core funnel to obtain a crude product and a filtrate A; recovering the filtrate A, and reusing the filtrate A in the alkali solution in the step 1);
3) purification and washing of the crude product: washing the crude product obtained in the step 2) with 0.1-6 mol/L KOH solution for 4-10 times to dissolve potassium ferrate, performing vacuum filtration by using a G2 glass sand core funnel to obtain a filtrate B, collecting the filtrate B, and performing vacuum filtration by using a G4 glass sand core funnel to obtain a filtrate C; then adding the filtrate C into a KOH solution with the temperature of 0 ℃ and the mol/L of 14, wherein the volume ratio of the filtrate C to the KOH solution is 1: 3-1: 5, and stirring for 5-30 minutes to separate out potassium ferrate crystals; quickly vacuum filtering the mixture by using a G3 glass sand core funnel to obtain K2FeO4Crystals and filtrate D; recovering the filtrate D, and recycling the filtrate D for the alkali solution in the step 1); then K is put2FeO4Leaching the crystal by using normal hexane, pentane and methanol respectively for four times in sequence, and leaching by using diethyl ether for two times;
4) and (3) drying: k after impurity removal2FeO4Vacuum drying the crystal at 60 deg.c for 12 hr to obtain potassium ferrate crystal with quality purity of 80-95.5%.
2. The method for preparing potassium ferrate by using the steel pickling waste liquid according to claim 1, which is characterized in that: the iron and steel pickling waste liquid in the step 1) contains Fe2+0.1-20% by mass of Fe3+0.1-20% by mass of Cl-The mass percentage of the acid is 0.1-35%, and the acidity is 0-6 mol/l.
3. The method for preparing potassium ferrate by using the steel pickling waste liquid according to claim 1, which is characterized in that: the alkali solution in the step 1) is a NaOH solution or a KOH solution, and the concentration of the alkali solution is 1-20 mol/L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101249905A CN100418890C (en) | 2006-11-09 | 2006-11-09 | Method for preparing potassium ferrate by using waste liquid from acid washing steel |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101249905A CN100418890C (en) | 2006-11-09 | 2006-11-09 | Method for preparing potassium ferrate by using waste liquid from acid washing steel |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1958462A true CN1958462A (en) | 2007-05-09 |
| CN100418890C CN100418890C (en) | 2008-09-17 |
Family
ID=38070332
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006101249905A Expired - Fee Related CN100418890C (en) | 2006-11-09 | 2006-11-09 | Method for preparing potassium ferrate by using waste liquid from acid washing steel |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100418890C (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102653437A (en) * | 2011-09-20 | 2012-09-05 | 卢玉柱 | Method for treating yellow sludge obtained in neutralization of steel pickling waste water lime |
| CN104828920A (en) * | 2015-05-18 | 2015-08-12 | 陈雷 | Preparation method of poly ferric perchloride flocculant |
| CN108503167A (en) * | 2018-03-30 | 2018-09-07 | 江苏宝钢精密钢丝有限公司 | A method of utilizing iron and steel pickling waste liquid synthesizing new water purification agent |
| CN108751380A (en) * | 2018-06-19 | 2018-11-06 | 怀化学院 | A kind of processing method of phase chromatography-use methanol waste water |
| CN113582236A (en) * | 2021-08-30 | 2021-11-02 | 陕西省石油化工研究设计院 | Preparation method of potassium ferrate |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1266819A (en) * | 1999-03-11 | 2000-09-20 | 中国科学院生态环境研究中心 | Flocculant of polyiron chloride prepared from waste hydrochloric acid as pickling liquid of iron and steel and its preparing process |
| CN1741206A (en) * | 2005-09-02 | 2006-03-01 | 卢玉柱 | Production of nano iron oxide black magnetic fluid with iron and steel hydrochloric acid pickling waste liquor |
| CN100532261C (en) * | 2005-11-03 | 2009-08-26 | 深圳职业技术学院 | Process for preparing solid potassium ferrate |
-
2006
- 2006-11-09 CN CNB2006101249905A patent/CN100418890C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102653437A (en) * | 2011-09-20 | 2012-09-05 | 卢玉柱 | Method for treating yellow sludge obtained in neutralization of steel pickling waste water lime |
| CN102653437B (en) * | 2011-09-20 | 2013-07-17 | 卢玉柱 | Method for treating yellow sludge obtained in neutralization of steel pickling waste water lime |
| CN104828920A (en) * | 2015-05-18 | 2015-08-12 | 陈雷 | Preparation method of poly ferric perchloride flocculant |
| CN108503167A (en) * | 2018-03-30 | 2018-09-07 | 江苏宝钢精密钢丝有限公司 | A method of utilizing iron and steel pickling waste liquid synthesizing new water purification agent |
| CN108751380A (en) * | 2018-06-19 | 2018-11-06 | 怀化学院 | A kind of processing method of phase chromatography-use methanol waste water |
| CN113582236A (en) * | 2021-08-30 | 2021-11-02 | 陕西省石油化工研究设计院 | Preparation method of potassium ferrate |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100418890C (en) | 2008-09-17 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105060579B (en) | A kind of method of advanced treating fluoride waste | |
| CN105236623B (en) | A kind of processing method of H acid waste water | |
| CN102583951B (en) | Acid lixiviation based recycling treatment method of aluminum circulating coagulation sludge | |
| CN102634673B (en) | Method for deeply removing iron ions from chromium-containing waste residue pickle liquor | |
| CN100465110C (en) | Coking waste water reuse treatment method | |
| CN105126742B (en) | A kind of method using modified kaolin sorbent treatment fluoride waste | |
| CN105923850A (en) | Treatment technology of refuse leachate membrane concentration liquid | |
| CN103787537B (en) | A kind for the treatment of process of sewage and application thereof | |
| CN109046229B (en) | Lanthanum hydroxide modified hydroxyapatite material and preparation method and application thereof | |
| CN102464440B (en) | Method for carrying out decrement on physicochemical and biochemical mixed sludge | |
| CN110255728A (en) | A kind of a new combined process method and system of landfill leachate treatment | |
| CN106145451A (en) | A kind of processing method of waste water containing thallium | |
| CN115043545B (en) | Magnetic flocculation coupling photocatalysis water purifying method and magnetic flocculation coupling photocatalysis water purifying device | |
| CN1958462A (en) | Method for preparing potassium ferrate by using waste liquid from acid washing steel | |
| CN101570355B (en) | Method for recovering inorganic coagulant in sewage sludge | |
| CN111320316A (en) | Landfill leachate membrane concentrated solution treatment method | |
| CN101215031A (en) | Method for preparing clay composite flocculant | |
| CN102515385B (en) | Treating technology for removing sodium from high sodium salt wastewater and device thereof | |
| CN1233561C (en) | Method for preparing polymeric ferric sulfate by using partial oxidation process | |
| CN109516537A (en) | Medicament, preparation method and the sewage water treatment method of fluoride in a kind of removal sewage | |
| CN112456673B (en) | Method for improving biodegradability of organic silicon wastewater | |
| CN110467312B (en) | Recycling treatment process for white carbon black production wastewater | |
| CN110590024B (en) | Method for treating DSD acid oxidative condensation wastewater | |
| JP2003300095A (en) | Method and apparatus for sewage treatment | |
| CN111333215A (en) | Method for removing chemical oxygen demand of landfill leachate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20080917 Termination date: 20101109 |