CN114890638A - Resource utilization method of oil-and organic-containing Fenton iron mud - Google Patents
Resource utilization method of oil-and organic-containing Fenton iron mud Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F11/00—Treatment of sludge; Devices therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
- B09B3/70—Chemical treatment, e.g. pH adjustment or oxidation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/14—Sulfates
Abstract
A resource utilization method of oil-and organic-containing Fenton iron mud comprises the steps of adding concentrated sulfuric acid and sodium chlorate into the oil-and organic-containing Fenton iron mud for heating and dissolving; standing the reaction liquid, removing upper-layer oil stains and filtering filter residues; adopting active carbon to adsorb and purify the solution; reducing the purifying liquid with ferric iron by using waste scrap iron and reduced iron powder; adding ferrous oxide into the reduced ferrous sulfate solution to adjust the pH value; the invention discloses a method for preparing ferrous sulfate from Fenton iron mud, which comprises the following steps of crystallizing filtrate to obtain a ferrous sulfate product, preparing the Fenton iron mud into ferrous sulfate, solving the problem of solid waste resource utilization of the Fenton iron mud, and realizing sustainable development.
Description
Technical Field
The invention relates to the technical field of recycling treatment of solid wastes, in particular to a utilization method of oily and organic iron mud generated by a Fenton treatment technology.
Background
In recent years, Fenton oxidation technology, which utilizes Fe under acidic conditions, can be effectively used to treat industrial wastewater 2+ And H 2 O 2 The reaction generates hydroxyl free radical, the oxidation energy of the free radical is strong and is stronger than that of common oxidant, and organic compound can be oxidized to generate CO 2 And H 2 And O, thereby effectively removing organic matters in the wastewater.
When the Fenton method is used for treating organic wastewater, the method has incomparable advantages of other methods, and is successfully applied to the treatment of various industrial organic wastewater so far. However, in the later stage of treating wastewater by the Fenton method, alkali and a flocculating agent are generally added to adjust the pH value for flocculation, a certain amount of chemical sludge is generated, and the sludge can cause a lot of harm if the sludge is not properly treated.
The current methods for treating Fenton iron mud mainly comprise the following methods: firstly, direct landfill, but still have a lot of problems to appear at the in-process of landfill, not only wasted a large amount of iron element wherein, occupy a large amount of lands, can produce secondary pollution moreover, can take place various chemical changes and destroy the soil that the mankind relied on to live like a large amount of iron mud along with the time lapse, wherein absorbent organic matter is decomposed by the microorganism, produces the stink, produces bigger environmental problem. Secondly, the obtained iron mud is burnt to remove the organic matters in the iron mud, and after burning, the iron in the iron mud is basically converted into Fe 3 O 4 Or Fe 2 O 3 And then the iron mud is recycled. The method can realize the recycling of the iron mud, but organic matters can carry out secondary pollution on the atmosphere in the incineration process, and the incineration process can consume a large amount of energy. The third is the curing method, which is to introduce the contaminants into a certain stable solid crystal lattice through chemical reaction, or to directly incorporate the contaminants into an inert substrate through a physical process. After such treatment, the toxicity and the mobility of dangerous solid wastes can be greatly reduced, and the engineering property of the treated objects can be improved.
The Chinese patent application with publication number 103252340A discloses a method for resource utilization of Fenton iron mud, which comprises adding concentrated sulfuric acid into iron mud, reacting concentrated sulfuric acid with ferric hydroxide to form ferric iron in solution, adding waste iron filings to reduce ferric iron into ferrous sulfate solution, and crystallizing to obtain industrial ferrous sulfate product. The method can carry out resource treatment on the conventional Fenton iron mud, but is not suitable for treating the iron mud containing a large amount of oil stains and organic matters. Because the oil stain and the iron mud are completely separated in acid leaching, higher reaction temperature and longer reaction time are needed, otherwise, the separation of the oil stain and the iron mud is difficult to realize; the adsorbed organic matter remains in the solution when the acid is dissolved, and if no effective measures are taken, a part of the adsorbed organic matter is adsorbed in the industrial ferrous sulfate in the crystallization process, so that the quality of the finished ferrous sulfate is influenced.
Disclosure of Invention
The technical purpose of the invention is as follows: through the adjustment of the reaction reagent and the improvement of the treatment process steps, the Fenton iron mud containing oil stains and organic matters is recycled, so that a ferrous sulfate product with high purity and good quality is prepared, and the economic benefit is improved.
In order to solve the technical problems, the invention adopts the technical scheme that: a resource utilization method of oil-containing and organic matter type Fenton iron mud comprises the following steps:
(1) dissolution
Adding water, concentrated sulfuric acid and sodium chlorate into oil-and-organic-containing Fenton iron mud to be treated to enable the liquid-solid ratio of a reaction system to be (6-9): 1, placing the reaction system at the temperature of 80-90 ℃ for dissolution reaction until the deep red color in the reaction system is continuously faded, and enabling the pH value of a reaction product to be 0.5-1;
(2) oil removal
Standing the reaction product prepared in the step (1) for at least 60min to enable the reaction product to be separated into an upper grease layer, a middle solution layer and a lower precipitation layer, fishing out the upper grease layer from the top for recycling, and filtering the rest materials to obtain filter residue and filtrate for later use;
(3) adsorption with activated carbon
Adding active carbon into the filtrate obtained in the step (2) according to the addition amount of 10-20 g/L for adsorption and purification treatment, and then filtering the obtained solid-liquid mixture to obtain a purified solution for later use;
(4) reduction of trivalent iron
Measuring Fe in the purified solution prepared in the step (3) 3+ Adding waste scrap iron into the purified solution prepared in the step (3) according to the proportion of 1.1-1.3 times of the theoretical addition amount, carrying out primary reduction at the temperature of 50-70 ℃ for 60-120 min, then adding reduced iron powder into the purified solution, carrying out deep reduction at the temperature of 25-35 ℃ until the purified solution turns into light blue, and filtering to remove filter residues to prepare a reducing solution for later use;
(5) adjusting the pH value
Adding ferrous oxide powder into the reducing solution prepared in the step (4), adjusting the pH value of the solution to 1-5, stirring for 30-90 min until the solution becomes bright green, and filtering to remove filter residues to prepare a ferrous sulfate solution for later use;
(6) crystallization of
And (5) crystallizing the ferrous sulfate solution prepared in the step (5) to obtain the finished product ferrous sulfate.
Further, in the step (1), the water content of the oil-containing and organic-matter-type Fenton iron mud is 70-80%, and the oil-containing and organic-matter-type Fenton iron mud contains deep red oil stains, organic matters, iron hydroxide and calcium hydroxide.
Further, in the step (1), the addition amount of sodium chlorate in the oil-containing and organic matter type Fenton iron mud to be treated is 50-100 g/1 Kg.
Further, in the step (1), the time of the dissolution reaction is 80-150 min.
Further, in the step (2), a screen is used to recover the upper grease layer from the reaction product which has been allowed to stand for layering.
And (3) further, washing and drying the filter residue obtained in the step (2) to obtain solid calcium sulfate which can be recycled.
Further, in the step (4), the addition amount of the reduced iron powder is 1 to 2% by mass of the purified solution.
Further, in the step (6), the specific method of the crystallization treatment comprises the steps of concentrating the ferrous sulfate solution into a saturated solution, adding anhydrous ethanol with the volume of 1/8-1/12, fully and uniformly mixing, performing freeze crystallization for 6-18 hours at the temperature of 8-20 ℃ in a freeze crystallization mode, and filtering the obtained crystallization liquid to obtain the filter residue which is the finished product ferrous sulfate.
Has the advantages that:
1. the invention relates to a resource utilization method of oil-and organic-containing Fenton iron mud, which is characterized in that after the Fenton iron mud containing oil stains and organic matters is leached and dissolved by concentrated sulfuric acid and sodium chlorate, reaction liquid can be kept stand for layering, the upper-layer oil stains can be fished out for recycling production by the method, and filter residues at the bottom layer are mainly a byproduct CaSO with the grade of more than 85 percent 4 And the solution of the middle layer can be used for producing high-purity ferrous sulfate. The whole treatment process can not generate new solid waste, and oil stain can be recycled and the byproduct CaSO 4 The method has the advantages of certain economic value, higher resource utilization degree and strong environmental friendliness when being sold.
2. According to the resource utilization method of the oil-and-organic-matter-containing Fenton iron mud, a small amount of sodium chlorate is added while concentrated sulfuric acid is added for leaching in the process of dissolving the Fenton iron mud. The addition of the sodium chlorate can promote the dissolution reaction in the reaction system and remove part of organic matters in the Fenton iron mud, so that the final ferrous sulfate product has high purity. The filtrate after oil stain removal is purified by adopting activated carbon adsorption, so that the mother liquor after crystallization and filtration can be directly recycled for production, no new wastewater is generated, and the resource utilization rate is high.
3. The quality of the ferrous sulfate obtained after the treatment of the iron mud can reach the standard of national standard GB664-93 chemical analysis purity, the Fenton iron mud is changed into valuable, and obvious economic benefit and social benefit are generated. The process is simple and easy to implement, is easy to industrialize, and has great popularization and application values.
Drawings
FIG. 1 is a schematic diagram of the process of the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the present invention will be described in further detail with reference to the accompanying drawings and specific embodiments. The described embodiments are only some, but not all embodiments 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. It should be noted that the embodiments and features of the embodiments in the present application may be arbitrarily combined with each other without conflict.
The invention relates to a resource utilization method of oil-and organic-containing Fenton iron mud, wherein the used Fenton iron mud raw material is Fenton iron mud containing oil stains and organic matters generated by workshop wastewater treatment, the water content of the Fenton iron mud is 70-80%, and other components mainly comprise dark red oil stains, organic matters, ferric hydroxide and calcium hydroxide. The specific treatment process comprises the following steps:
(1) dissolving: adding a proper amount of water, concentrated sulfuric acid and a small amount of sodium chlorate into Fenton iron mud generated by workshop wastewater treatment containing oil and organic matters, wherein the adding amount of the concentrated sulfuric acid is to control the final pH value of a reaction system to be within 0.5-1, the adding amount of the sodium chlorate is 50-100 g of 1Kg of wet iron mud, after the water is added, the liquid-solid ratio of the reaction system is 6-9: 1, after the water is completely added, placing the reaction system at the temperature of 80-90 ℃ for carrying out dissolution reaction for 80-150 min until the crimson in the reaction system is continuously faded out, and when the crimson of the reaction liquid is basically faded out, the reaction approaches the end point;
(2) oil removal: standing the reaction solution obtained in the step (1) for 60min, and obviously dividing the reaction solution into 3 layers: taking out the upper layer of oil sludge from the upper layer of the oil sludge by using a screen, filtering to obtain filtrate and filter residue, wherein the filter residue is mainly calcium sulfate slag, and the filtrate is mainly ferric sulfate solution;
(3) activated carbon adsorption: because the filtrate prepared in the step (2) contains a large amount of organic matters, such as phenol and benzene compounds, petroleum and many other artificial compounds, the solution can be further purified by using activated carbon adsorption, and the adding amount of the activated carbon in the filtrate is 10-20 g per liter of the filtrate;
(4) reducing ferric iron: reducing the filtrate which is used for removing most organic matters in the step (3) by using waste iron filings, wherein the addition amount of the waste iron filings is 1.1-1.3 times of the theoretical dosage, the reduction temperature of the waste iron filings is 50-70 ℃, the reduction time is 60-120 min, adding a small amount of reduced iron powder into the solution after reduction, and carrying out deep reduction at the temperature of 25-35 ℃ until the solution is light blue, namely the reduction end point;
(5) adjusting the pH value of the solution: adding ferrous oxide powder into the reduced ferrous sulfate solution to adjust the pH of the solution to 1-5, stirring for 30-90 min, and filtering to obtain a pure ferrous sulfate solution, wherein the solution is a bright green end point;
(6) and (3) crystallization: concentrating the ferrous sulfate solution obtained in the step (5) into a saturated solution, adding anhydrous ethanol with the volume of 1/8-1/12 into the saturated solution, fully and uniformly mixing, performing freeze crystallization for 6-18 hours at the temperature of 8-20 ℃ in a freeze crystallization mode, and filtering the obtained crystal liquid to obtain filter residues, namely the finished product ferrous sulfate.
The invention adopts Fenton iron mud containing oil and organic matters as raw materials to prepare high-purity ferrous sulfate and CaSO 4 The by-products and the recyclable oil stains solve the problem of solid waste resource utilization of the Fenton iron mud and realize sustainable development.
Example 1
In this example, the amount of wet iron mud is 442.27g, the water content of the wet iron mud is 80%, during treatment, 300ml of water is added to the wet iron mud, a certain amount of concentrated sulfuric acid is added, the pH value at the end of the reaction is controlled to be about 0.5, and in order to ensure that the reaction is relatively thorough, 40g of sodium chlorate is additionally added to promote the reaction. Other conditions of the reaction are: the reaction temperature is 90 ℃, and the reaction time is 80 min. After the reaction is finished, the reaction liquid is divided into three parts, wherein the upper layer is waste oil, the middle layer is an iron-containing solution, and the lower layer is slightly white slag. And fishing out the upper oil stain layer by using a screen mesh for recycling, and then filtering to obtain filtrate and filter residue, wherein the filter residue is mainly calcium sulfate residue, and the filtrate is mainly ferric sulfate.
The filter residue is washed with water, dried and weighed, the weight is 98.17g, and the filter residue is produced as a byproduct.
500ml of the filtrate was added with 10g of activated carbon, and adsorption was carried out at room temperature. Filtering after adsorption, and reducing the filtrate by adopting waste scrap iron and reduced iron powder. The reduction process is divided into two steps, the first step is pre-reduction, and the reduction process is as follows: at 50 deg.C, scrap iron is added to reduce the solution to light yellow. And the second step is deep reduction, namely, adding reduced iron powder with the mass of 1-2% into the supernatant at the temperature of 30 ℃, and finally, neutralizing, adding ferrous oxide powder into the reduced ferrous sulfate solution to adjust the pH of the solution to 1, stirring for 90min, and then, obtaining the pure ferrous sulfate solution after filtering, wherein the solution becomes light green.
The crystallization process of the solution is as follows: firstly, concentrating the solution to saturation, then adding 80ml of absolute ethyl alcohol, crystallizing at the temperature of 20 ℃, crystallizing for 12 hours, and then filtering the obtained crystal liquid to obtain filter residue, namely the finished ferrous sulfate crystal.
Example 2
In the embodiment, the using amount of the wet iron mud is 453.53g, the water content of the wet iron mud is 70%, 300ml of water is firstly added into the wet iron mud during treatment, a certain amount of concentrated sulfuric acid is then added, the pH value of the reaction is controlled to be about 0.9 after the reaction is finished, and in order to ensure that the reaction is relatively thorough, 23g of sodium chlorate is additionally added to promote the reaction. Other conditions of the reaction are: the reaction temperature is 80 ℃, and the reaction time is 150 min. After the reaction is finished, the reaction liquid is divided into three parts, wherein the upper layer is waste oil, the middle layer is an iron-containing solution, and the lower layer is slightly white slag. And fishing out the upper oil stain layer by using a screen mesh for recycling, and then filtering to obtain filtrate and filter residue, wherein the filter residue is mainly calcium sulfate residue, and the filtrate is mainly ferric sulfate.
The residue was washed with water, dried and weighed to a weight of 103.99g, and was produced as a by-product.
520ml of the filtrate was added with 6g of activated carbon, and adsorption was carried out at room temperature. Filtering after adsorption, and reducing the filtrate by adopting waste scrap iron and reduced iron powder. The reduction process is divided into two steps, the first step is pre-reduction, and the reduction process is as follows: at 70 ℃, waste scrap iron is added to reduce the solution into light yellow. And the second step is deep reduction, namely, adding reduced iron powder with the mass of 1-2% into the supernatant at 25 ℃, and finally neutralizing, adding ferrous oxide powder into the reduced ferrous sulfate solution to adjust the pH of the solution to 3, stirring for 60min, and then, obtaining the pure ferrous sulfate solution, wherein the solution becomes light green, and the end point is obtained by filtering.
The crystallization process of the solution is as follows: firstly, concentrating the solution to saturation, then adding 50ml of absolute ethyl alcohol, crystallizing at the temperature of 8 ℃ for 18h, and then filtering the obtained crystal liquid to obtain filter residue, namely the finished ferrous sulfate crystal.
Example 3
In the embodiment, the using amount of wet iron mud is 500g, the water content of the wet iron mud is 75%, 350ml of water is added into the wet iron mud during treatment, a certain amount of concentrated sulfuric acid is added, the pH value of the reaction is controlled to be about 0.7 after the reaction is finished, and in order to ensure that the reaction is relatively thorough, 50g of sodium chlorate is additionally added to promote the reaction. Other conditions of the reaction are: the reaction temperature is 85 ℃, and the reaction time is 100 min. After the reaction is finished, the reaction liquid is divided into three parts, wherein the upper layer is waste oil, the middle layer is an iron-containing solution, and the lower layer is slightly white slag. And fishing out the upper oil stain layer by using a screen mesh for recycling, and then filtering to obtain filtrate and filter residue, wherein the filter residue is mainly calcium sulfate residue, and the filtrate is mainly ferric sulfate.
The residue was washed with water, dried and weighed to a weight of 123.38g, and was produced as a by-product.
680ml of filtrate was added to the reaction solution, and the mixture was adsorbed on activated carbon (13.6 g) at room temperature. Filtering after adsorption, and reducing the filtrate by adopting waste scrap iron and reduced iron powder. The reduction process is divided into two steps, the first step is pre-reduction, and the reduction process is as follows: at 60 ℃, waste scrap iron is added to reduce the solution into light yellow. And the second step is deep reduction, namely, adding reduced iron powder with the mass of 1-2% into the supernatant at 35 ℃, and finally neutralizing, adding ferrous oxide powder into the reduced ferrous sulfate solution to adjust the pH of the solution to 5, stirring for 30min, and then, obtaining the pure ferrous sulfate solution, wherein the solution becomes light green, and the end point is obtained by filtering.
The crystallization process of the solution is as follows: firstly, concentrating the solution to saturation, then adding 100ml of absolute ethyl alcohol, crystallizing at the temperature of 17 ℃ for 8 hours, and then filtering the obtained crystal liquid to obtain filter residue, namely the finished ferrous sulfate crystal.
The above embodiments are merely to illustrate the technical solutions of the present invention and not to limit the present invention, and the present invention has been described in detail with reference to the preferred embodiments. It will be understood by those skilled in the art that various modifications and equivalent arrangements may be made without departing from the spirit and scope of the present invention and it should be understood that the present invention is to be covered by the appended claims.
Claims (8)
1. A resource utilization method of oil-containing and organic matter type Fenton iron mud is characterized by comprising the following steps:
(1) dissolution
Adding water, concentrated sulfuric acid and sodium chlorate into oil-and-organic-containing Fenton iron mud to be treated to enable the liquid-solid ratio of a reaction system to be (6-9): 1, placing the reaction system at the temperature of 80-90 ℃ for dissolution reaction until the deep red color in the reaction system is continuously faded, and enabling the pH value of a reaction product to be 0.5-1;
(2) oil removal
Standing the reaction product prepared in the step (1) for at least 60min to separate the reaction product into an upper grease layer, a middle solution layer and a lower precipitate layer, fishing out the upper grease layer from the top for recycling, and filtering the rest materials to obtain filter residue and filtrate for later use;
(3) adsorption with activated carbon
Adding active carbon into the filtrate obtained in the step (2) according to the addition amount of 10-20 g/L for adsorption and purification treatment, and then filtering the obtained solid-liquid mixture to obtain a purified solution for later use;
(4) reduction of trivalent iron
Measuring Fe in the purified solution prepared in the step (3) 3+ Adding waste scrap iron into the purified solution prepared in the step (3) according to the proportion of 1.1-1.3 times of the theoretical addition amount, carrying out primary reduction at the temperature of 50-70 ℃ for 60-120 min, then adding reduced iron powder into the purified solution, carrying out deep reduction at the temperature of 25-35 ℃ until the purified solution turns into light blue, and filtering to remove filter residues to prepare a reducing solution for later use;
(5) adjusting the pH value
Adding ferrous oxide powder into the reducing solution prepared in the step (4), adjusting the pH value of the solution to 1-5, stirring for 30-90 min until the solution becomes bright green, and filtering to remove filter residues to prepare a ferrous sulfate solution for later use;
(6) crystallization of
And (5) crystallizing the ferrous sulfate solution prepared in the step (5) to obtain the finished product ferrous sulfate.
2. The resource utilization method of the oil-and-organic-containing Fenton iron mud as claimed in claim 1, wherein: in the step (1), the water content of the oil-containing and organic-matter-type Fenton iron mud is 70-80%, and the oil-containing and organic-matter-type Fenton iron mud contains deep red oil stains, organic matters, iron hydroxide and calcium hydroxide.
3. The resource utilization method of the oil-and-organic-containing Fenton iron mud as claimed in claim 1, wherein: in the step (1), the addition amount of sodium chlorate in the oil-containing and organic-matter-type Fenton iron mud to be treated is 50-100 g/1 Kg.
4. The resource utilization method of the oil-and-organic-containing Fenton iron mud as claimed in claim 1, wherein: in the step (1), the dissolving reaction time is 80-150 min.
5. The resource utilization method of the oil-and-organic-containing Fenton iron mud as claimed in claim 1, wherein: in the step (2), a screen is used to recover the upper grease layer from the reaction product which is layered after standing.
6. The resource utilization method of the oil-and-organic-containing Fenton iron mud as claimed in claim 1, wherein: and (3) washing and drying the filter residue obtained in the step (2) to obtain solid calcium sulfate which can be recycled.
7. The resource utilization method of the oil-and-organic-containing Fenton iron mud as claimed in claim 1, wherein: in the step (4), the addition amount of the reduced iron powder is 1-2% of the mass of the purification solution.
8. The resource utilization method of the oil-and-organic-containing Fenton iron mud as claimed in claim 1, wherein: in the step (6), the specific method of the crystallization treatment is that the ferrous sulfate solution is concentrated into a saturated solution, then absolute ethyl alcohol with the volume of 1/8-1/12 is added into the saturated solution, the mixture is fully mixed, then a freezing crystallization mode is adopted, freezing crystallization is carried out for 6-18 hours at the temperature of 8-20 ℃, then the obtained crystallization liquid is filtered, and the obtained filter residue is the finished ferrous sulfate.
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