CN110665362A - Method for preparing desulfurizer by utilizing Fenton iron mud - Google Patents
Method for preparing desulfurizer by utilizing Fenton iron mud Download PDFInfo
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- CN110665362A CN110665362A CN201910981713.3A CN201910981713A CN110665362A CN 110665362 A CN110665362 A CN 110665362A CN 201910981713 A CN201910981713 A CN 201910981713A CN 110665362 A CN110665362 A CN 110665362A
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- desulfurizer
- iron mud
- fenton iron
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/81—Solid phase processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/48—Sulfur compounds
Abstract
The invention relates to the technical field of desulfurization, and particularly discloses a preparation method of a desulfurizing agent. The method takes dehydrated Fenton iron mud as a main raw material, adds a certain amount of binder and pore-forming agent, and adopts an extrusion molding roasting method to prepare the desulfurizer. According to the method, pH is not required to be adjusted, reagents which are easy to cause secondary pollution such as acid, alkali and complexing agents are not used, and the fenton iron mud can be prepared into the desulfurizer with excellent effect only by adopting the adhesive and the pore-forming agent which are low in cost, so that the fenton iron mud can be recycled. The desulfurizer prepared by the invention takes ferric oxide as a main component, has higher sulfur capacity, high sulfur absorption weight gain rate and high sulfur absorption speed; after high-temperature roasting, the desulfurizer has high strength, long service life, high crushing strength and wide application range. And the desulfurizer has high desorption rate, is renewable and has a simple regeneration method.
Description
Technical Field
The invention relates to the technical field of desulfurization, in particular to a preparation method of a desulfurizing agent.
Background
The Fenton oxidation method is an efficient and economic advanced wastewater oxidation technology, and hydrogen peroxide and ferrous ions react under an acidic condition to generate hydroxyl radicals (OH) with strong oxidizing property so as to oxidize pollutants in wastewater into CO2And H2And O, thereby effectively removing organic matters in the wastewater. The Fenton oxidation method has the advantages of strong oxidation capacity, simple equipment, easy operation, low operation cost and the like, and is widely applied to industrial wastewater treatment in the industries of chemical industry, papermaking, printing and dyeing, pharmacy and the like.
However, in the fenton oxidation process, ferrous iron is oxidized into ferric iron, and a large amount of fenton iron mud is generated in the subsequent pH adjustment process, and the fenton iron mud is often treated as dangerous solid waste, so that the subsequent treatment cost is increased, and the fenton oxidation process becomes one of important factors restricting the popularization and development of the fenton technology.
In the industrial production processes of coal chemical industry, smelting and the like, sulfur-containing gas which seriously pollutes the environment can be generated, the existence of the sulfur-containing gas can not only corrode a pipeline, but also possibly poison the used catalyst, so that the service life of the catalyst is reduced. The iron oxide desulfurizer is commonly used in industrial production for removing hydrogen sulfide, and although the raw materials of iron and iron oxide are relatively low in cost, the consumption of the desulfurizer is continuously increased, and the production cost of enterprises is also increased. Therefore, the method for preparing the desulfurizer by using the Fenton iron mud as the raw material can effectively solve the problem of handling the Fenton iron mud, effectively utilize iron resources and reduce the cost of industrial production such as coal chemical industry, smelting and the like.
Chinese patent ZL201410397289.5 discloses a comprehensive recycling method of Fenton iron mud, which is characterized in that Fenton iron mud is acidified and dissolved, and is added with complexing agent and sodium alkali to be used for absorbing hydrogen sulfide. However, the method consumes a large amount of acid, alkali and complexing agent, is easy to generate secondary pollution, and is complicated to control in the actual operation process.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to provide a method for preparing a desulfurizer by utilizing fenton iron mud. By adopting the method, the problem that Fenton iron mud is difficult to dispose can be solved, and the desulfurizer which is low in cost, convenient and fast to apply and good in regeneration performance is prepared in a resource recycling mode.
The Fenton iron mud is a mixture which is generated by Fenton and Fenton-like processes and takes iron-based hydroxide or iron-based oxide as a main component.
The invention realizes the aim through the following technical scheme:
according to the first aspect, the invention provides a method for preparing a desulfurizer by utilizing Fenton iron mud.
Further, the method comprises the steps of:
(1) adjusting the water content of Fenton iron mud to 15% -30%;
(2) adding an adhesive and a pore-forming agent into the Fenton iron mud obtained in the step (1), and uniformly stirring to obtain a mixed material;
the mass ratio of the addition amount of the adhesive to the dehydrated Fenton iron mud is 8: 100-25: 100;
the mass ratio of the addition amount of the pore-forming agent to the dehydrated Fenton iron mud is 0.05: 100-0.15: 100;
(3) adjusting the humidity of the mixed material to be 8-15%, and extruding and granulating to obtain a desulfurizing agent prefabricated material with the particle size of 3-10 mm;
(4) and roasting the preformed material of the desulfurizer at 380-300 ℃ for 2-4 h to obtain the desulfurizer.
Wherein, the adhesive is CaO and/or MgO.
Wherein the pore-forming agent is selected from NaHCO3、KHCO3、NH4HCO3And starch.
Furthermore, according to practical applications, in the step (2), a binder, a pore-forming agent, a reinforcing agent and/or a catalytic assistant can be optionally added into the fenton iron mud obtained in the step (1), and the mixture is uniformly stirred to obtain a mixed material.
Wherein the mass ratio of the addition amount of the reinforcing agent to the dehydrated Fenton iron mud is 1: 100-20: 100; such enhancers include, but are not limited to, CaSO4、Na2SO4Gypsum, white cement and water glass.
Wherein the mass ratio of the addition amount of the catalytic promoter to the dehydrated Fenton iron mud is 0.1: 100-2: 100; the catalytic promoter is one or more of manganese, copper, cobalt, nickel, zinc, vanadium, cerium and lanthanum metal powder and salts and oxides thereof.
In step (3) of the above process of the present invention, a flat-die pelletizer is used for extrusion pelletization.
In a second aspect, the present invention provides a desulfurizing agent, which is prepared by the method of the present invention.
The desulfurizer prepared by the preparation method of the invention uses the main component of Fe (OH)3The Fenton iron mud is extruded and formed under the action of a bonding agent, and is converted into Fe after being roasted at high temperature under the action of a pore-forming agent2O3Or Fe3O4To form the desulfurizing agent rich in pores.
The desulfurizer prepared by the method has the specific gravity of 380-1000 kg/m3The pore volume is 0.4-0.3 mL/g (namely the volume of micropores in the desulfurizer per unit weight), the strength is more than or equal to 80N, and the saturated working sulfur capacity is more than or equal to 40%. Compared with the existing desulfurizer, the desulfurizer has the advantages of higher sulfur absorption rate, higher crushing strength and longer service life.
The invention has the beneficial effects that:
the invention develops a method for preparing a desulfurizer by utilizing Fenton iron mud, which does not need to adjust pH, does not use reagents which are easy to generate secondary pollution, such as acid, alkali, complexing agents and the like, and can prepare the Fenton iron mud into the desulfurizer with excellent effect only by adopting a bonding agent and a pore-forming agent with low cost, thereby realizing the reutilization of the Fenton iron mud.
The desulfurizer produced by the method takes ferric oxide as a main component, has higher sulfur capacity, high sulfur absorption weight gain rate and high sulfur absorption speed; after high-temperature roasting, the desulfurizer has high strength, long service life, high crushing strength and wide application range. And the desulfurizer has high desorption rate, is renewable and has a simple regeneration method.
The method avoids the possible environmental pollution caused by improper treatment of the Fenton iron mud, reduces the treatment cost of the Fenton iron mud, has low additive cost and lower production cost, and is suitable for industrial large-scale production.
Detailed Description
The invention provides a method for preparing a desulfurizer by utilizing Fenton iron mud.
The method specifically comprises the following steps:
(1) adjusting the water content of Fenton iron mud to 15% -30%;
(2) adding an adhesive and a pore-forming agent into the Fenton iron mud obtained in the step (1), and uniformly stirring to obtain a mixed material;
the mass ratio of the addition amount of the adhesive to the dehydrated Fenton iron mud is 8: 100-25: 100;
the mass ratio of the addition amount of the pore-forming agent to the dehydrated Fenton iron mud is 0.05: 100-0.15: 100;
(3) adjusting the humidity of the mixed material to be 8-15%, and extruding and granulating to obtain a desulfurizing agent prefabricated material with the particle size of 3-10 mm;
(4) and roasting the preformed material of the desulfurizer at 380-300 ℃ for 2-4 h to obtain the desulfurizer.
Specifically, in the step (1), the water content of the fenton iron mud is generally 90% to 99%, and the step needs to perform dehydration treatment on the fenton iron mud to reduce the water content of the fenton iron mud to 15% to 30%; the dehydration can be carried out by adopting the modes of centrifugation, natural air drying, heating and the like, and the dehydration mode is not limited in the invention.
Further, in the step (2), the binder of the present invention is CaO and/or MgO; in one embodiment of the invention, the binder is CaO; in another embodiment of the present invention, the binder is MgO; in another embodiment of the present invention, the binder is CaO and MgO.
Further, in the step (2), the pore-forming agent is selected from NaHCO3、KHCO3、NH4HCO3And starch; in one embodiment of the present invention, the pore former is NaHCO3(ii) a In another embodiment of the present invention, the pore-forming agent is KHCO3(ii) a In another embodiment of the present invention, the pore-forming agent is NH4HCO3(ii) a In another embodiment of the present invention, the pore former is starch; in another embodiment of the present invention, the pore former is NaHCO3And KHCO3(ii) a In another embodiment of the present invention, the pore-forming agent is NH4HCO3And starch.
Further, according to practical application, a certain amount of reinforcing agent and catalytic assistant can be selectively added in the step (2) for fully mixing and stirring;
for example, preferably, when the requirement on the mechanical strength of the desulfurizer is high, 1-20 parts by mass of a reinforcing agent is added, so that the strength of the desulfurizer can be improved; when synchronous denitration is needed, 0.1-2 parts by mass of catalytic assistant are added to realize synchronous desulfurization and denitration; the mass part is the dosage of the reinforcing agent or the catalytic assistant relative to 100 mass parts of dehydrated Fenton iron mud;
wherein the enhancer includes but is not limited to CaSO4、Na2SO4Gypsum and white cementWater glass, etc.; the catalytic promoter is one or more of manganese, copper, cobalt, nickel, zinc, vanadium, cerium and lanthanum metal powder and salts and oxides thereof.
Further, in the step (3), the humidity of the mixture may be adjusted by using tap water or air drying (heating). Setting the particle size of the desulfurizer pre-preparation to be 3-10 mm from the aspects of roasting heat transfer and application convenience; after the mixture is adjusted to be proper, the fully and uniformly stirred mixture is extruded and granulated by a flat-die granulator.
Further, in the step (4), the roasting temperature is 380-300 ℃, the roasting process is constant temperature heating or gradient temperature rising, preferably gradient temperature rising, and the roasting time is 2-4 hours.
The desulfurizer prepared by the preparation method of the invention uses the main component of Fe (OH)3The Fenton iron mud is extruded and formed under the action of a bonding agent, and is converted into Fe after being roasted at high temperature under the action of a pore-forming agent2O3Or Fe3O4To form the desulfurizing agent rich in pores.
The desulfurizer prepared by the method has the specific gravity of 380-1000 kg/m3The pore volume is 0.4-0.3 mL/g (namely the volume of micropores in the desulfurizer per unit weight), the strength is more than or equal to 80N, and the saturated working sulfur capacity is more than or equal to 40%. Compared with the existing desulfurizer, the desulfurizer has the advantages of higher sulfur absorption rate, higher crushing strength and longer service life.
Therefore, it should be understood that the desulfurizing agent prepared by the method of the present invention also belongs to the protection scope of the present invention.
The raw materials or reagents involved in the invention are all common commercial products, and the operations involved are all routine operations in the field unless otherwise specified.
The above-described preferred conditions may be combined with each other to obtain a specific embodiment, in accordance with common knowledge in the art.
Preferred embodiments of the present invention will be described in detail with reference to the following examples. It is to be understood that the following examples are given for illustrative purposes only and are not intended to limit the scope of the present invention. Various modifications and alterations of this invention will become apparent to those skilled in the art without departing from the spirit and scope of this invention.
The experimental procedures used in the following examples are all conventional procedures unless otherwise specified.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
Example 1
This example is used to illustrate a method for preparing a desulfurizing agent from fenton iron sludge, and specifically includes the following steps:
(1) the water content of Fenton iron mud with the water content of 98 percent is reduced to 30 percent by adopting a natural air drying mode;
(2) 100 parts by mass of fenton iron mud with a water content of 30% was taken, and 15 parts by mass of CaO (binder) and 0.15 part by mass of NH were added thereto4HCO3(pore-forming agent) and 2 parts by mass of gypsum (reinforcing agent) are fully and uniformly stirred;
(3) adjusting the humidity of the mixed material to be 12%, and extruding and granulating by using a flat die granulator with the aperture of 3mm to obtain a desulfurizer prefabricated material with the particle size of 3 mm;
(4) roasting at 420 deg.c for 2.5 hr to obtain the desulfurizing agent.
The detection shows that the pore volume of the desulfurizer is 0.53mL/g, the saturation working sulfur capacity is 54%, and the strength reaches more than 90N.
Example 2
This example is used to illustrate a method for preparing a desulfurizing agent from fenton iron sludge, and specifically includes the following steps:
(1) dewatering Fenton iron mud with the water content of 98% to about 70% by adopting a plate-and-frame filter press, and reducing the water content to 30% by heating;
(2) 100 parts by mass of fenton iron mud with a water content of 30% is taken, 10 parts by mass of CaO and 10 parts by mass of MgO (composite binder) are added, and 0.05 part by mass of NaHCO is added3(pore-forming agent), 10 parts by mass of water glass (reinforcing agent), 2 parts by mass of Mn (NO)3)2(catalytic assistant), fully stirring uniformly;
(3) adding a small amount of water to adjust the humidity of the mixed material to be 15%, and extruding and granulating by using a flat-die granulator with the aperture of 8mm to obtain a desulfurizer prefabricated material with the particle size of 8 mm;
(4) roasting at 400 ℃ for 1h, heating to 500 ℃ for 1h, continuing to heat to 300 ℃ for 1h, and obtaining the desulfurizer.
The detection shows that the pore volume of the desulfurizer is 0.48mL/g, the saturation working sulfur capacity is 45%, and the strength reaches more than 95N.
Example 3
This example is used to illustrate a method for preparing a desulfurizing agent from fenton iron sludge, and specifically includes the following steps:
(1) dewatering Fenton iron mud with the water content of 98% by adopting a plate-and-frame filter press until the water content is about 70%, and reducing the water content to about 20% by heating;
(2) taking 100 parts by mass of Fenton iron mud with the water content of 20%, adding 10 parts by mass of MgO (composite adhesive) and 0.08 part by mass of starch (pore-forming agent) into the Fenton iron mud, and fully and uniformly stirring the mixture;
(3) adjusting the humidity of the mixed material to be 8%, and extruding and granulating by using a flat-die granulator with the aperture of 3mm to obtain a desulfurizer prefabricated material with the particle size of 3 mm;
(4) roasting at 380 deg.c for 4 hr to obtain the desulfurizing agent.
The detection shows that the pore volume of the desulfurizer is 0.40mL/g, the saturation working sulfur capacity is 48%, and the strength reaches more than 80N.
Experimental example 1
This experimental example is intended to illustrate the desorption efficiency of the desulfurizing agent prepared by the method of the present invention.
The regeneration is carried out by adopting a natural ventilation method, and the reaction principle is as follows:
Fe2O3+H2S→Fe2S3+H2O
Fe2S3+O2→Fe2O3+S
in this experiment, H-containing gas was continuously introduced into the desulfurizing agent2S mixed gas to be imported and exported H2Stable S concentrationAnd (3) changing the time, namely the desulfurizing agent reaches adsorption saturation, taking out the desulfurizing agent with the adsorption saturation, standing for 48 hours under a natural ventilation condition, and measuring the sulfur capacity of the desulfurizing agent, wherein the sulfur capacity is reduced within 5%.
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (10)
1. A method for preparing a desulfurizer by utilizing Fenton iron mud is characterized in that the Fenton iron mud is used as a main raw material, a binder and a pore-forming agent are added, then extrusion granulation is carried out, and high-temperature roasting molding is carried out, so that the desulfurizer with iron oxide as a main component is obtained.
2. Method according to claim 1, characterized in that it comprises the following steps:
(1) adjusting the water content of Fenton iron mud to 15% -30%;
(2) adding an adhesive and a pore-forming agent into the Fenton iron mud obtained in the step (1), and uniformly stirring to obtain a mixed material;
the mass ratio of the addition amount of the adhesive to the dehydrated Fenton iron mud is 8: 100-25: 100;
the mass ratio of the addition amount of the pore-forming agent to the dehydrated Fenton iron mud is 0.05: 100-0.15: 100;
(3) adjusting the humidity of the mixed material to be 8-15%, and extruding and granulating to obtain a desulfurizing agent prefabricated material with the particle size of 3-10 mm;
(4) and roasting the preformed material of the desulfurizer at 380-300 ℃ for 2-4 h to obtain the desulfurizer.
3. The method according to claim 2, wherein the binder is CaO and/or MgO.
4. The method of claim 2, wherein the pore former is selected from NaHCO3、KHCO3、NH4HCO3And starch.
5. The method according to any one of claims 2 to 4, wherein in the step (2), a binder, a pore-forming agent, a reinforcing agent and/or a catalytic assistant are added to the Fenton iron mud obtained in the step (1), and the mixture is uniformly stirred to obtain a mixed material.
6. The method according to claim 5, wherein the mass ratio of the addition amount of the reinforcing agent to the dehydrated Fenton iron mud is 1: 100-20: 100; such enhancers include, but are not limited to, CaSO4、Na2SO4Gypsum, white cement and water glass.
7. The method according to claim 5, wherein the mass ratio of the addition amount of the catalytic promoter to the dehydrated Fenton iron mud is 0.1: 100-2: 100; the catalytic promoter is one or more of manganese, copper, cobalt, nickel, zinc, vanadium, cerium and lanthanum metal powder and salts and oxides thereof.
8. A method according to any one of claims 2 to 4 or 3 to 7, wherein in step (3), extrusion granulation is carried out using a flat die granulator.
9. A desulfurizing agent, characterized in that the desulfurizing agent is prepared by the method of any one of claims 1 to 8.
10. The desulfurizing agent according to claim 9, wherein the specific gravity of the desulfurizing agent is 380-1000 kg/m3The pore volume is 0.4-0.3 mL/g, the strength is more than or equal to 80N, and the saturated working sulfur capacity is more than or equal to 40%.
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| CN113372964A (en) * | 2021-06-28 | 2021-09-10 | 中晶环境科技股份有限公司 | Preparation method of iron oxide-based desulfurizing agent and application of composition |
| CN114920433A (en) * | 2022-05-31 | 2022-08-19 | 新宇药业股份有限公司 | Method for recycling chemical iron mud generated in antibiotic wastewater treatment |
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