CN109956536B - Reactive filter material for coking wastewater treatment and preparation and use methods thereof - Google Patents
Reactive filter material for coking wastewater treatment and preparation and use methods thereof Download PDFInfo
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
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- C—CHEMISTRY; METALLURGY
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/705—Reduction by metals
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Abstract
A filter material with reactivity comprises the following raw materials in proportion: coking coke powder: hot rolling of iron scale: blast furnace fly ash =1 to 2: 1 to 3: 1; and (3) adding a binder, wherein the adding amount of the binder is according to the total volume of the three raw materials: binder =1: 1 to 3; the particle size of the coking coke powder is 100-200 meshes, the particle size of the blast furnace dust removal ash is 100-200 meshes, and the particle size of the hot-rolled iron sheet is 0.5-2 mm. The preparation method comprises the following steps: pretreatment of raw materials: uniformly mixing the pretreated raw materials according to a ratio; adding a binder; granulating; drying; and sintering for later use. The using method comprises the following steps: the filter reactor filled with the filter material is placed before or after the biochemical treatment of the coking wastewater or placed before and after the biochemical treatment of the coking wastewater simultaneously. The invention ensures that the coking wastewater treatment meets the requirements, fully utilizes the resource of the iron-containing and carbon-containing waste, and the filter material can return to the sintering process after the reaction without the problem of secondary pollution.
Description
Technical Field
The invention relates to a material used in coking wastewater treatment and a preparation and use method thereof, and particularly belongs to a reactive filter material used in coking wastewater treatment and a preparation and use method thereof.
Background
A large amount of iron-containing metallurgical wastes can be generated in the ferrous metallurgy process, such as iron scale generated in the steel rolling process, blast furnace dust generated in the blast furnace smelting process and the like. The steel rolling iron scale is iron-containing oxide generated on the surface of steel products after rolled pieces are rapidly cooled when meeting water in the rolling process of a steel rolling mill, the generation amount of the iron scale accounts for about 3-5 percent of the processed steel products, taking an annual 1000-ten thousand-ton steel enterprise as an example, the iron scale generated in the rolling process is about 9-ten thousand tons every year, the iron content in the rolled iron scale is up to 80-90 percent, the rolled iron scale is waste residue with the highest iron content in various iron-containing waste residues of the steel enterprise, and the iron exists mainly in the form of FeO and Fe3O4And Fe2O3And the like. Heald for rolling iron sheet at presentThe combined utilization mainly comprises returning to factories for use (can return to sintering, ironmaking or steelmaking for use as raw materials), manufacturing ferrosilicon alloy, preparing iron-containing raw materials in the chemical industry and the like.
In the iron-making process: the blast furnace dust is dust discharged along with blast furnace gas in the iron making process, and the amount of the dust generated by each ton of iron is 20-60 kg. The blast furnace dust generally contains 25-45% of carbon and 15-30% of iron. At present, flotation, gravity separation and magnetic separation methods are mostly adopted for comprehensive utilization of the fly ash, iron, carbon and other substances in the fly ash are mainly recovered, and a large amount of waste is still discarded.
In addition to ferrous metallurgical wastes, a large amount of carbonaceous wastes, such as coking fly ash, is also produced in the coking process. The coking fly ash is dust particles obtained by treating a large amount of smoke dust generated in the coking process during coal charging, coke discharging and coke quenching by corresponding dust removal equipment in the coking production process, and is mainly characterized by high organic matter content, fine particles, small specific gravity and easy accumulation to pollute the surrounding environment. At present, the research and application of the coking dedusting ash mainly comprises replacing clean coal to be used for blast furnace coal injection, pressing to form moulded coal and blending coal for coking, blending in sintered ore, preparing active carbon and the like.
Coking wastewater is industrial wastewater which is difficult to biodegrade and is generated in the processes of high-temperature dry distillation of coal, gas purification and byproduct recovery, wherein the industrial wastewater contains oils, volatile phenols, aromatic hydrocarbons, heterocyclic compounds such as oxygen, sulfur, nitrogen and the like, cyanogen, sulfur, thiocyanogen, metal salts such as iron, magnesium and sodium and the like, and is typical industrial wastewater which is difficult to treat.
At present, the coking wastewater is treated by a biological method, a coagulation method, an advanced oxidation method and other processes, but the treatment cost is high, and the treatment cost is hard to bear by many enterprises, but the treatment is not required from the environmental protection perspective. This forces the skilled person to continue the innovative work. As retrieved: in the aspect of coking wastewater treatment, the four-stage coking wastewater in Bao Steel chemical industry adopts an A/A/O biochemical treatment, ultrafiltration, nanofiltration and reverse osmosis three-membrane deep treatment process, the coking wastewater in saddle steel chemical industry adopts an A/A/O biochemical treatment, ozone catalytic oxidation and biological filter deep treatment process, a coking plant of Jingtang iron and steel company adopts an A/O/O biochemical treatment, electrocatalytic oxidation, electrocoagulation, electro-flotation, ultrafiltration and reverse osmosis two-membrane deep treatment process, and a tai steel coking company adopts an A/A/O biochemical treatment and MBR treatment process. The technical combination has the problems of high investment and operation cost, and is unacceptable for general enterprises. In the aspect of preparation of reactive filter materials, retrieval shows that most of the materials adopt reduced iron powder, zinc powder, activated carbon powder, clay and the like as raw materials to prepare the reactive filter material, but the raw materials all adopt finished products, so that the preparation cost is high, and when the reactive filter material is used for treating coking wastewater, the treatment cost of the wastewater cannot be reduced even if a good use effect can be ensured; in addition, in most of the articles or patents, when the preparation of the reactive filter material is involved, the adopted raw materials such as zinc, clay and the like have great harm to the sintering and iron-making processes due to new elements and silicon elements, and the filter material cannot return to the sintering or iron-making processes after being used, so that the use cost is increased invisibly. Therefore, the invention adopts the ferrous and carbonaceous waste of the ferrous metallurgy process to prepare the reactive filter material for treating the coking wastewater, thereby not only reducing the wastewater treatment cost, but also returning the filter material after reaction to the sintering or iron-making process for recycling.
The invention applies the metallurgical iron-containing waste to the coking wastewater treatment process, namely, hot-rolled iron scale, blast furnace dust removal ash and coking coke powder are used as raw materials to prepare a reactive filter material which is used for coking biochemical pretreatment to improve the biodegradability of wastewater, and can also be used for further removing organic matters in water after biochemical treatment, thereby not only reducing the coking wastewater treatment cost, but also achieving the purpose of fully recycling the iron-containing carbon-containing waste to be comprehensively utilized, and the filter material after reaction can be further returned to the sintering process in the metallurgical process system.
Disclosure of Invention
The invention aims to prepare a reactive filter material for coking wastewater treatment by utilizing metallurgical iron-containing and carbon-containing wastes, and provides the reactive filter material for coking wastewater treatment, which can reduce the coking wastewater treatment cost, can fully and comprehensively utilize the iron-containing and carbon-containing wastes after reaction and can return the filter material to a sintering process on the basis of ensuring that the coking wastewater treatment meets the requirements, and the preparation and use methods thereof.
The measures for realizing the aim are as follows:
a filter material with reactivity comprises the following raw materials: the coke powder, the rolled iron scale and the blast furnace dust are prepared from the following three raw materials in percentage by volume: coking coke powder: hot rolling of iron scale: blast furnace fly ash 1 to 2: 1 to 3: 1; and (3) adding a binder in the following proportion of the volume total amount of the three raw materials: binder 1:1 to 3; the particle size of the coking coke powder is 100-200 meshes, the particle size of the blast furnace dust removal ash is 100-200 meshes, and the particle size of the rolled iron scale is 0.5-2 mm.
It is characterized in that: the binder consists of deionized water, starch and calcium lignosulfonate, and the addition proportion is as follows according to the volume ratio: deionized water: starch: calcium lignosulfonate 1:0.1 to 0.2.
Further: the volume ratio of the raw materials of the filter material is as follows: coking coke powder: hot rolling of iron scale: blast furnace fly ash is 1: 1.2 to 2: 1.35 to 2.85.
It is characterized in that: the rolling scale is scale produced by hot rolling or scale produced by silicon steel rolling or both
A preparation method of a filter material with reactivity comprises the following steps:
1) pretreatment of raw materials:
A. and (3) processing rolled iron oxide scales: washing the rolled iron scale with the particle size of 0.5-2 mm after screening with water for at least two times until water-soluble salt substances and impurities in the iron scale are removed;
stirring and soaking by using 1-5 mol/LNaOH alkali liquor for not less than 12 h;
after solid-liquid separation, washing the solid again with water to remove impurities, and reserving the solid for later use;
B. pretreating blast furnace dust: firstly, washing the blast furnace dust with the particle size of 0.15-0.30 mm after screening to remove water-soluble salt substances and impurities in the blast furnace dust;
stirring and soaking by using 1-5 mol/LNaOH alkali liquor for not less than 12 h;
after solid-liquid separation, washing the solid again with water to remove impurities, and reserving the solid for later use;
C. pretreating the coke powder: taking coke powder with the particle size of 0.15-0.30 mm in the coking procedure, and washing with water to remove impurities for later use;
2) the three pretreated raw materials are mixed according to the following ratio: hot rolling of iron scale: blast furnace fly ash is 1:1 to 2: 1 to 3 are mixed evenly;
3) the following steps are performed according to deionized water: starch: adding the uniformly mixed binder into the mixture obtained in the step 2) according to the volume ratio of 1: 0.1-0.2 of calcium lignosulfonate, and uniformly stirring for later use; the volume total of the three raw materials is as follows: binder 1:1 to 3, adding and uniformly stirring;
4) and (3) granulating: preparing spherical particles with the particle size of 5-10 mm;
5) and (3) drying: drying the spherical particles at normal temperature for not less than 24 h;
6) sintering: sintering in the air isolation condition, wherein the sintering temperature is 1000-1200 ℃, the sintering time is 2-4 h, and the sintering atmosphere is nitrogen protection reducing atmosphere, so as to prepare the reactive filter material for later use.
A method for using a reactive filter material comprises the following steps:
1) placing the filter material made by claim 5 in a filtration reactor until full;
2) and placing the filter reactor filled with the filter material before or after the biochemical treatment of the coking wastewater or simultaneously before and after the biochemical treatment of the coking wastewater.
It is characterized in that: the used filter material is used as an iron-containing raw material in a sintering process.
According to the invention, the particle size of the coking coke powder is controlled to be 0.15-0.3 mm, the particle size of the blast furnace dust is controlled to be 0.15-0.3 mm, and the particle size of the rolled iron scale is controlled to be 0.5-2 mm, so that the quality of the iron-containing and carbon-containing waste raw material is controlled based on the actual condition of each raw material, and the iron-containing and carbon-containing waste raw material can be fully mixed during preparation and prepared into a uniform material mutually wrapped during sintering.
The invention uses 1-5 mol/LNaOH alkali liquor to stir and soak, the stirring and soaking time is not less than 12h, so as to fully remove oil substances carried by the dust, and avoid the pollution of waste gas generated during high-temperature sintering to the environment.
The atmosphere of the invention adopts nitrogen when sintering, because the nitrogen can isolate air when protecting, and ensure the reducing atmosphere, the iron element in the iron scale can be reduced to zero-valent iron in the presence of carbon element, and the invention has reactivity, which is determined by adopting the iron scale as the raw material.
Compared with the prior art, the method can reduce the treatment cost of the coking wastewater on the basis of ensuring that the coking wastewater treatment meets the requirements, can achieve the aim of fully and comprehensively utilizing the iron-containing and carbon-containing wastes, and can return the filter material to the sintering process after the reaction, so that the problem of secondary pollution is solved.
Detailed Description
The present invention is described in detail below:
example 1:
a filter material with reactivity comprises the following raw materials: the coke powder, the rolled iron scale and the blast furnace dust are prepared from the following three raw materials in percentage by volume: coking coke powder: hot rolling of iron scale: blast furnace fly ash is 1: 1: 1; and (3) adding a binder in the following proportion of the volume total amount of the three raw materials: binder 1: 1.3; the particle size of the coking coke powder is 100-200 meshes, the particle size of the blast furnace dust removal ash is 100-200 meshes, and the particle size of the rolled iron scale is 0.5-2 mm.
The preparation method comprises the following steps:
1) pretreatment of raw materials:
crushing and screening silicon steel scale, taking particles with the particle size of 0.5-1 mm after screening, washing for many times to remove salt and impurities till the particles are clean, and stirring and soaking the particles in 2mol/LNaOH alkali liquor for 12 hours; washing the solid after solid-liquid separation with water again to remove impurities till the solid is clean for later use;
taking blast furnace dust with the particle size of 100-150 meshes after screening, washing with water to remove salt and impurities until the dust is clean, stirring and soaking the dust in 2mol/LNaOH alkali liquor for 12 hours, and washing the solid after solid-liquid separation with water again to remove impurities for cleaning and standby;
taking coke powder with the granularity of 100-150 meshes in the coking process, and washing with water to remove impurities until the coke powder is clean for later use;
uniformly mixing the three pretreated raw materials according to the proportion as follows: the particle size of the coke powder is 100-150 meshes: silicon steel oxide scale with granularity of 0.5-1 mm: the blast furnace dust removal ash with the granularity of 100-150 meshes is 1: 1:1, mixing uniformly;
2) adding a binder according to the volume total of the three raw materials: binder 1: 2;
the composition of the binder is as follows: mixing starch: calcium lignosulfonate: stirring and mixing deionized water in a volume ratio of 0.1:0.1:1 until the deionized water is uniform, and preparing liquid for later use;
3) adding the liquid prepared in the step 2) into the mixture which is pretreated and uniformly mixed in the step 1), wherein the volume ratio of the mixture to the liquid is 1:2, and uniformly stirring;
kneading into spherical granules with particle diameters of 2.5mm, 3.0mm and 3.5 mm;
4) drying the spherical particles for 24 hours at normal temperature, sintering the dried spherical particles under the condition of air isolation, wherein the sintering temperature is 1000 ℃, the sintering time is 2 hours, and then performing nitrogen protection to obtain the reactive filter material.
The using method comprises the following steps:
the prepared spherical particles are placed in a filtering reactor to be full, and are placed in a pretreatment before the biochemical treatment of the coking wastewater, and the spherical particles are used for the incoming water of the coking wastewater and flow through a filter filled with the filter material after the quality and the quantity of the incoming water are adjusted.
The used filter material is sent to a sintering process and used as a raw material of the sintering process.
The prepared reactive filter material is used for the biochemical pretreatment equipment of the coking wastewater: the diameter of the filter is 5m, the height of the filter is 3.6m, the water quantity is 150 tons/hour, the calculated empty tower flow rate is 0.3mm/s, the actual flow rate is about 1mm/s, and the residence time in the filter is about 1 h. The coking ammonia distillation wastewater is homogenized by the regulating tank and then enters a filter filled with the filter material.
The relevant indexes of the filter in the embodiment are shown in table 1:
TABLE 1 the filter material of this example was used in the coking biochemical pretreatment
Example 2:
a filter material with reactivity comprises the following raw materials: the coke powder, the rolled iron scale and the blast furnace dust are prepared from the following three raw materials in percentage by volume: coking coke powder: hot rolling of iron scale: blast furnace fly ash 1.2: 1.6: 1; and (3) adding a binder in the following proportion of the volume total amount of the three raw materials: binder 1: 2.1; the particle size of the coking coke powder is 100-200 meshes, the particle size of the blast furnace dust removal ash is 100-200 meshes, and the particle size of the rolled iron scale is 0.5-2 mm.
The preparation method comprises the following steps:
1) pretreatment of raw materials:
crushing and screening silicon steel scale, taking particles with the particle size of 1-2 mm after screening, washing for many times to remove salt and impurities till the particles are clean, and stirring and soaking the particles in alkali liquor with the concentration of 3.5mol/LNaOH for 24 hours; washing the solid after solid-liquid separation with water again to remove impurities till the solid is clean for later use;
taking blast furnace dust with the particle size of 150-200 meshes after screening, washing with water to remove salt and impurities until the dust is clean, stirring and soaking in 3.5mol/LNaOH alkali liquor for 24 hours, and washing the solid after solid-liquid separation with water again to remove impurities for cleaning for later use;
taking coke powder with the granularity of 150-200 meshes in a coking process, and washing with water to remove impurities until the coke powder is clean for later use;
uniformly mixing the three pretreated raw materials according to the proportion as follows: the particle size is 150-200 meshes of coke powder: silicon steel scale with granularity of 1-2 mm: the blast furnace dust removal ash with the granularity of 150-200 meshes is 1.2: 1.6: 1, mixing uniformly;
2) adding a binder according to the volume total of the three raw materials: binder 1:2.1, carrying out;
the composition of the binder is as follows: mixing starch: calcium lignosulfonate: stirring and mixing deionized water in a volume ratio of 0.16:0.14:1 until the deionized water is uniform, and preparing liquid for later use;
3) adding the liquid prepared in the step 2) into the mixture which is pretreated and uniformly mixed in the step 1), wherein the volume ratio of the mixture to the liquid is 1:2.1, and uniformly stirring;
kneading into spherical granules with particle diameters of 4mm, 4.5mm and 5 mm;
4) drying the spherical particles for 48h at normal temperature, sintering the dried spherical particles under the condition of air isolation, wherein the sintering temperature is 1100 ℃, the sintering time is 3h, and then performing nitrogen protection to obtain the reactive filter material.
The using method comprises the following steps:
and (3) placing the prepared spherical particles in a filtering reactor to be full, placing the spherical particles in coking wastewater after biochemical treatment and before advanced treatment, enabling the effluent of the coking ammonia distillation wastewater after adjustment, biochemical treatment and coagulating sedimentation to enter a filter filled with the filler, and enabling the effluent of the filter to enter a subsequent ozone oxidation advanced treatment unit after hydraulic retention time of 60 min.
The relevant indexes of the filter water inlet and outlet are shown in the table 2, and the water used for the coking wastewater flows through the filter filled with the filter material after the water quality and the water quantity are adjusted.
The used filter material is sent to a sintering process and used as a raw material of the sintering process.
The prepared reactive filter material is used for the biochemical pretreatment equipment of the coking wastewater: the diameter of the filter is 5m, the height of the filter is 3.6m, the water quantity is 150 tons/hour, the calculated empty tower flow rate is 0.3mm/s, the actual flow rate is about 1mm/s, and the residence time in the filter is about 1 h. The coking ammonia distillation wastewater is homogenized by the regulating tank and then enters a filter filled with the filter material.
The relevant indexes of the filter in the embodiment are shown in the following table 2:
the prepared reactive filter material is used for the advanced treatment of coking wastewater after biochemical treatment, the effluent of the coking ammonia distillation wastewater after adjustment, biochemical treatment and coagulating sedimentation enters a filter filled with the filler, the hydraulic retention time is 60min, and the effluent of the filter enters a subsequent ozone oxidation advanced treatment unit. The relevant indexes of the filter water inlet and outlet are shown in the table 2:
TABLE 2 the filter material of this example is used for coking biochemical post-treatment
Claims (6)
1. A reactive filter material for treating coking wastewater comprises the following raw materials: the coke powder, the rolled iron scale and the blast furnace dust are prepared from the following three raw materials in percentage by volume: coking coke powder: hot rolling of iron scale: blast furnace fly ash =1 to 2: 1 to 3: 1; and (3) adding a binder in the following proportion of the volume total amount of the three raw materials: binder =1: 1 to 3; the particle size of the coked coke powder is 100-150 meshes, the particle size of the blast furnace dust is 100-150 meshes, and the particle size of the rolled iron scale is 0.5-2 mm;
the binder consists of deionized water, starch and calcium lignosulfonate, and the addition proportion is as follows according to the volume ratio: deionized water: starch: calcium lignosulfonate =1: 0.1 to 0.2.
2. The reactive filter material for the treatment of coking wastewater of claim 1, wherein: the volume ratio of the raw materials of the filter material is as follows: coking coke powder: hot rolling of iron scale: blast furnace fly ash =1: 1.2 to 2: 1.
3. the reactive filter material for the treatment of coking wastewater of claim 1, wherein: the hot-rolled iron oxide scale is produced by hot rolling.
4. The method for preparing the reactive filter material for the coking wastewater treatment according to claim 1 comprises the following steps:
1) pretreatment of raw materials:
A. and (3) processing rolled iron oxide scales: washing the rolled iron scale with the particle size of 0.5-2 mm after screening with water for at least two times until water-soluble salt substances and impurities in the iron scale are removed;
stirring and soaking by using 1-5 mol/LNaOH alkali liquor for not less than 12 h;
after solid-liquid separation, washing the solid again with water to remove impurities, and reserving the solid for later use;
B. pretreating blast furnace dust: firstly, washing the screened blast furnace dust with the particle size of 100-150 meshes with water to remove water-soluble salt substances and impurities in the blast furnace dust;
stirring and soaking by using 1-5 mol/LNaOH alkali liquor for not less than 12 h;
after solid-liquid separation, washing the solid again with water to remove impurities, and reserving the solid for later use;
C. pretreating the coke powder: taking coke powder with the particle size of 100-150 meshes in the coking procedure, and washing with water to remove impurities for later use;
2) the three pretreated raw materials are mixed according to the following ratio: hot rolling of iron scale: blast furnace fly ash =1 to 2: 1 to 3: 1, uniformly mixing in proportion;
3) the following steps are performed according to deionized water: starch: adding the binder uniformly mixed according to the volume ratio of calcium lignosulfonate =1: 0.1-0.2 into the mixture obtained in the step 2), and uniformly stirring the mixture for later use; the volume total of the three raw materials is as follows: binder =1: 1 to 3, adding and uniformly stirring;
4) and (3) granulating: preparing spherical particles with the particle size of 5-10 mm;
5) and (3) drying: drying the spherical particles at normal temperature for not less than 24 h;
6) sintering: sintering in the air isolation condition, wherein the sintering temperature is 1000-1200 ℃, the sintering time is 3-4 h, and the sintering atmosphere is nitrogen protection reducing atmosphere, so as to prepare the reactive filter material for later use.
5. The use method of the reactive filter material for the treatment of the coking wastewater, which is characterized by comprising the following steps:
1) placing a filter material having reactivity according to claim 1 in a filtration reactor until full;
2) the filter reactor filled with the filter material is arranged before or after the biochemical treatment of the coking wastewater.
6. The use method of the reactive filter material for the treatment of the coking wastewater according to claim 5, characterized in that: the used filter material is used as an iron-containing raw material in a sintering process.
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| JPS5441550A (en) * | 1977-09-07 | 1979-04-02 | Nippon Kokan Kk <Nkk> | Method of treating dust collecting drain in iron mill |
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| CN104276840A (en) * | 2013-07-03 | 2015-01-14 | 济南大学 | Blast furnace dusted ash based particle electrode and preparation method thereof |
| CN104310553A (en) * | 2014-10-31 | 2015-01-28 | 武汉钢铁(集团)公司 | Resource utilization method of blast furnace dust |
| CN104310535A (en) * | 2014-10-31 | 2015-01-28 | 武汉钢铁(集团)公司 | Resource utilization method of blast furnace dust and coke furnace dust |
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