CN105854784A - Method for preparing environmental protection material used for sewage treatment by reforming metallurgical dregs - Google Patents
Method for preparing environmental protection material used for sewage treatment by reforming metallurgical dregs Download PDFInfo
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Abstract
The invention relates to a method for preparing an environmental protection material used for sewage treatment by reforming metallurgical dregs. The method is characterized in that solid waste slag discharged by metallurgy industry is taken as a raw material, through acid dissolution and filtering, a raw material solution is obtained, the pH value is adjusted, and the steps of hydro-thermal synthesis, washing, drying and grinding are carried out to prepare the environmental protection material. The material used for processing printing and dyeing sewage, cation red decolourization rate percent is greater than 90%; when the material is used for processing heavy metal sewage, Cr(VI) clearance is greater than 85%, Cu<2+> clearance is greater than 90%, and VO3<-> clearance is greater than 90%; when the material is used for processing phosphorus-containing sewage, the phosphor clearance is greater than 85%. The method has the advantage that the raw material is the solid waste slag, the environmental protection material is prepared, the environmental protection material has good application value, can realize slag high value utilization. The method uses the waste slag to prepare the environmental protection material, so that printing and dyeing, heavy metal and phosphorus-containing sewage can be purified, and the method has good economic benefit and wide industrial application prospect.
Description
Technical field
The invention belongs to bulk solid waste higher value application field, utilize metallurgical slag to reform particularly to one and prepare environmental protection merit
The method of energy material and the application in sewage disposal, i.e. application in dyeing and printing sewage processes, such as cationic red X-FRL；?
Application in heavy metal containing sewage process, such as Cr (VI), Cu2+、VO3 -；Application in phosphorus-containing wastewater processes, such as H2PO4 -。
Background technology
Slag is the waste residue produced in metallurgical industry, and its generation rate is the 8%-15% of crude steel yield, and " 12 " period is to 2015
Year crude steel yield by about 700,000,000 tons measuring and calculating, metallurgical slag year industry amount and treating capacity will be more than 300,000,000 tons.Therefore, iron and steel enterprise's waste residue
Process and recycling problem the most increasingly come into one's own.Country's " 12 " development plan just has been pointed out, metallurgical slag
Comprehensive utilization ratio strive reaching more than 73%.Wherein the comprehensive utilization ratio of blast furnace slag reaches more than 86%, and slag reaches 60%, ferrum
Fe alloy slag reaches 60%.But, the present situation of China's comprehensive utilization at present differs greatly with this planning, especially have " poor-quality water
Mud grog " the utilization rate of converter slag of title be only 10%-20%.The slag that domestic iron and steel enterprises produces can not process in time,
Cause big steel slag land occupation, pollute environment.But the most unavailable solid waste of slag, wherein contain substantial amounts of slag steel,
The available components such as calcium oxide, ferrum and magnesium oxide.So, for making iron and steel enterprise create economy and environmental benefit, it is suitable to select
Process technique and utilization ways to develop the recycle value of slag be the most necessary and urgent.
The approach of steel slag utilization is a lot, and CN103849695A discloses the processing method of a kind of slag, and the method is included in can
FeO in slag is aoxidized and generates Fe3O4Under conditions of, molten state slag is contacted with oxygen-containing gas, described oxygenous
During in body, amount of oxygen makes slag, the FeO oxidation of more than 80% generates Fe3O4；Then the steel after contacting with oxygen-containing gas
Slag carries out cooling down, crushes, sieves and magnetic separation, obtains Armco magnetic iron.By this kind of method, can not only effectively reclaim in slag
Full ferrum, promote slag value, additionally it is possible to the waste residue obtained is efficiently used in concrete.CN103553454A
Disclose and a kind of utilize slag make admixture and make the preparation method of high performance concrete of aggregate.Concrete is by Binder Materials, bone
Material, water reducer and mixing water composition；Binder Materials is composited by cement, slag micro powder and slag micropowder；Slag micro powder used,
The specific surface area of slag micropowder controls respectively 400～600m2/ kg, 400～500m2/kg；Aggregate is by rubble, Steel-slag Sand and river sand
Composition；The particle diameter of Steel-slag Sand is 5～10mm, and part substitutes rubble, and its volume is 20%～50%；High efficiency water reducing agent is previously dissolved in
Water, mixes with mixing water.The method can prepare C20～C60 grade concrete, improves the comprehensive utilization ratio of slag；Gained coagulation
Soil service behaviour, mechanical property each side are all good, and durability be improved significantly.Although the utilization ways of slag is more,
But higher value application is such as applied and there is no report at solid base houghite.Traditionally, hydrotalcite-like materials preparation is usually
Utilize chemicals finished product, such as magnesium nitrate hexahydrate, ANN aluminium nitrate nonahydrate, iron chloride etc..Containing Determination of multiple metal elements in slag,
Reformation prepares whether novel environment friendly functional material houghite can possess good absorption as material prepared by chemicals finished product
Must study Deng performance number.
There are the features such as interlayer exchangeable anions, intercalation function and memory effect due to houghite, may be used for sewage disposal,
It is adsorbent that CN101269870 reports with LDHs, removes the Phos in waste water by absorption and ion exchange, but
Its LDHs is prepared by pure salt, and interlayer anion is OH-, halogen, NO3-；CN102863042A discloses utilization printing and dyeing
Anionic dye in waste water, the LDHs that will be added in water makes organic hydrotalcite while processing this waste water, chemical industry simultaneously
Organic substance in organic wastewater is adsorbed to hydrotalcite layers, together removes with pollutant；CN103394328A discloses one
The preparation method and application technology of Hydroxyl-functionalized Ionic Liquids/hydrotalcite-like composite material, main employing coprecipitation prepares neatly
Stone, is used for removing bisphenol-A in water, phenol or nonyl phenol pollutant.CN103638905A, CN101653717A report
The absorption of LDHs heavy metal copper, hydrargyrum, lead and cadmium, but LDHs is pure salt and prepares, and overwhelming majority technology is still for now
It is in development.
With solid waste slag as raw material, reformation prepares environment-friendly function material houghite for sewage disposal, the treatment of wastes with processes of wastes against one another,
Big steel slag can be solved pile up land occupation, pollute the problem of environment, the sewage disposal of wider range can be used for again, make solid
Garbage obtains higher value application, economic and environment-friendly.
Summary of the invention
Present invention is to be solved be technical problem is that: provide a kind of metallurgical slag reformation to prepare the new method of environment-friendly function material,
It is mainly used in printing and dyeing, heavy metal, the process of the sewage such as phosphorous, it is achieved the treatment of wastes with processes of wastes against one another.
Technical scheme is as follows:
The environment-friendly function material method for sewage disposal is prepared in a kind of metallurgical slag reformation that the present invention provides, and comprises the following steps:
(1) slag is placed in beaker with certain mass ratio with acid, dissolves under uniform temperature；
(2) solidliquid mixture step (1) obtained filters, and obtains filtrate；
(3) filtrate (2) obtained, with Ca (OH)2Solid or NaOH solid regulation PH to 8-13, obtain suspension；
(4) suspension 100-200 DEG C (3) obtained, Hydrothermal Synthesis 6-50h, washing is centrifuged to neutrality, obtains solid；
(5) solid 80-200 DEG C (4) obtained is dried, and grinds and obtains powder.
(6) powder (5) obtained processes for dyeing and printing sewage, such as cationic red X-FRL sewage；
(7) powder (5) obtained processes for heavy metal containing sewage, as containing Cr (VI), Cu2+, VO3 -Heavy metal containing sewage；
(8) powder (5) obtained processes for phosphorus-containing wastewater, as containing H2PO4 -Sewage；
(9) the powder roasting (5) obtained, clearance has a certain amount of raising.
Preferably, in step (1), acid include organic acid (acetic acid, benzoic acid, heteropoly acid) and mineral acid (hydrochloric acid, nitric acid,
Sulphuric acid, sulfurous acid, phosphoric acid), acid concentration is 2-6mol/L；
Preferably, in step (1), acid solution and slag mass ratio are 10-40, and acid solubility temperature is 70-120 DEG C；
Preferably, in step (3), PH=8-13；
Preferably, in step (4), hydrothermal synthesizing condition is 100-200 DEG C, 6-50h；
Preferably, in step (5), baking temperature is 80-200 DEG C, and powder is functional material houghite, its cation M3+
For Fe3+、Al3+In one or both, M2+For Ca2+、Mg2+、Mn2+In one or both；
Preferably, in step (6), cationic red initial concentration is 5-100ppm, adsorbent amount 0.5-4g/L, adsorption temp
20-65 DEG C, time 0.5-4h；
Preferably, in step (7), Cr (VI) initial concentration is 3-100ppm, adsorbent amount 0.3-4g/L, adsorption temp
20-65 DEG C, time 0.3-6h；
Preferably, in step (7), Cu2+Initial concentration is 5-200ppm, adsorbent amount 0.6-6g/L, adsorption temp 20-80 DEG C,
Time 0.5-6h；
Preferably, in step (7), VO3 -Initial concentration is 5-300ppm, adsorbent amount 0.5-10g/L, adsorption temp 20-65 DEG C,
Time 0.5-20h；
Preferably, in step (8), H2PO4 -Initial concentration is 1-100ppm, adsorbent amount 0.5-5g/L, adsorption temp
20-65 DEG C, time 0.3-8h；
Object used by the present invention is the slag produced in steelmaking process, wherein contains calcium, ferrum, silicon, magnesium, aluminum and a small amount of manganese phosphorus etc.
Oxide, essential mineral be mutually tricalcium silicate, dicalcium silicate, monticellite, calcium and magnesium rhodonite, calcium aluminoferrite and
Silicon, magnesium, ferrum, manganese, the oxide of phosphorus, have a large amount of available component, for large industrial solid castoff.Slag hydro-thermal is closed
Become environmental protection functional material houghite, for sewage disposal, the treatment of wastes with processes of wastes against one another.Both solve big steel slag and pile up land occupation, dirt
The problem of dye environment, can be used for again printing and dyeing, the process of heavy metal, phosphorus-containing wastewater, makes solid waste obtain higher value application,
There is good economic benefit and wide industrial applications prospect.
Accompanying drawing explanation
Fig. 1 is functional material SEM collection of illustrative plates
Fig. 2 is functional material SEM collection of illustrative plates after roasting
Detailed description of the invention
Below in conjunction with example, patent of the present invention is further illustrated.
Embodiment 1.
The preparation method of environment-friendly function material is prepared in metallurgical slag reformation:
(1) by the acetic acid quality of slag and 5mol/L than 1:25,90 DEG C of oil bath stirring and dissolving, obtain solidliquid mixture；
(2) solidliquid mixture step (1) obtained filters, and obtains filtrate；
(3) filtrate (2) obtained is with Ca (OH)2Solid regulation PH to 12, obtains suspension；
(4) suspension 150 DEG C (3) obtained, Hydrothermal Synthesis 16h, washing is centrifuged to neutrality, obtains solid；
(5) solid 80 DEG C (4) obtained is dried, and pulverizes, obtains the functional material class that interlayer anion is acetate ion
Brucite.
Functional material prepared by the present embodiment application in the red dyeing and printing sewage of Liquidity limit:
Functional material 0.05g is put in the cationic red X-FRL sewage of 100mL50ppm, 46.3 DEG C of shaking table concussions, survey after 4h
Examination dye strength is 2.95ppm, and percent of decolourization is 94.1%.
Embodiment 2.
The preparation method of environment-friendly function material is prepared in metallurgical slag reformation:
(1) by the hydrochloric acid mass ratio 1:30 of slag Yu 3mol/L, 95 DEG C of oil bath stirring and dissolving, solidliquid mixture is obtained；
(2) solidliquid mixture step (1) obtained filters, and obtains filtrate；
(3) filtrate (2) obtained regulates PH to 11 with NaOH solid, obtains suspension；
(4) suspension 145 DEG C (3) obtained, Hydrothermal Synthesis 40h, washing is centrifuged to neutrality, obtains solid；
(5) solid 90 DEG C (4) obtained is dried, and pulverizes.
(6) the 450 DEG C of roasting 3h of powder (5) obtained, obtain functional material houghite.
Functional material prepared by the present embodiment application in Adsorption of Heavy Metals Cr (VI) sewage:
Being put into by functional material 0.2g in the Neutral potassium chromate sewage of 200mL60ppm, 65 DEG C of shaking table concussions, after 6h, test dye concentration is
6.756ppm, clearance is 88.74%.
Embodiment 3.
The preparation method of environment-friendly function material is prepared in metallurgical slag reformation:
(1) by the acetic acid quality of slag and 4mol/L than 1:35,105 DEG C of oil bath stirring and dissolving, obtain solidliquid mixture；
(2) solidliquid mixture step (1) obtained filters, and obtains filtrate；
(3) filtrate (2) obtained is with Ca (OH)2Solid regulation PH to 12.5, obtains suspension；
(4) suspension 150 DEG C (3) obtained, Hydrothermal Synthesis 20h, washing is centrifuged to neutrality, obtains solid；
(5) solid 80.5 DEG C (4) obtained is dried, and pulverizes, obtains the functional material that interlayer anion is acetate ion
Houghite.
Functional material prepared by the present embodiment is in Adsorption of Cu2+Application in sewage:
Functional material 0.1g is put into the Cu of 100mL80ppm2+In sewage, 35 DEG C of shaking table concussions, test dye concentration after 3h
For 6.76ppm, clearance rate is 91.55%.
Embodiment 4.
The preparation method of environment-friendly function material is prepared in metallurgical slag reformation:
(1) by the nitric acid mass ratio 1:35 of slag Yu 3mol/L, 85 DEG C of oil bath stirring and dissolving, solidliquid mixture is obtained；
(2) solidliquid mixture step (1) obtained filters, and obtains filtrate；
(3) filtrate (2) obtained regulates PH to 10 with NaOH solid, obtains suspension；
(4) suspension 140 DEG C (3) obtained, Hydrothermal Synthesis 10h, washing is centrifuged to neutrality, obtains solid；
(5) solid 70 DEG C (4) obtained is dried, and pulverizes, obtains the functional material class that interlayer anion is nitrate ion
Brucite.
Functional material prepared by the present embodiment is at absorption VO3 -Application in sewage:
Functional material 5g is put into the NaVO of 100mL200ppm3In sewage, 45 DEG C of shaking table concussions, after 10h, test dye is dense
Degree is 13.2ppm, and clearance rate is 93.4%.
Embodiment 5.
The preparation method of environment-friendly function material is prepared in metallurgical slag reformation:
(1) by the sulphuric acid mass ratio 1:40 of slag Yu 3.5mol/L, 110 DEG C of oil bath stirring and dissolving, solidliquid mixture is obtained；
(2) solidliquid mixture step (1) obtained filters, and obtains filtrate；
(3) filtrate (2) obtained regulates PH to 12.3 with NaOH solid, obtains suspension；
(4) suspension 145 DEG C (3) obtained, Hydrothermal Synthesis 15h, washing is centrifuged to neutrality, obtains solid；
(5) solid 78 DEG C (4) obtained is dried, and pulverizes, obtains the functional material class that interlayer anion is sulfate ion
Brucite.
Functional material prepared by the present embodiment application in processing phosphorus-containing wastewater:
Functional material 0.1g is put into the KH of 100mL50ppm2PO4In, 25 DEG C of shaking table concussions, after 4h, test dye concentration is
6.53ppm, clearance is 86.94%.
Claims (12)
1. an environment-friendly function material method for sewage disposal is prepared in metallurgical slag reformation, comprises the following steps:
(1) slag is placed in beaker with certain mass ratio with acid, dissolves under uniform temperature；
(2) solidliquid mixture step (1) obtained filters, and obtains filtrate；
(3) filtrate (2) obtained, with Ca (OH)2Solid or NaOH solid regulation PH to 8-13, obtain suspension；
(4) suspension 100-200 DEG C (3) obtained, Hydrothermal Synthesis 6-50h, washing, to neutral, obtains solid；
(5) solid 80-200 DEG C (4) obtained is dried, and grinds and obtains powder.
(6) powder (5) obtained processes for dyeing and printing sewage, such as cationic red X-FRL sewage；
(7) powder (5) obtained processes for heavy metal containing sewage, as containing Cr (VI), Cu2+, VO3 -Heavy metal containing sewage；
(8) powder (5) obtained processes for phosphorus-containing wastewater, as containing H2PO4 -Sewage；
(9) the powder roasting (5) obtained, clearance has a certain amount of raising.
2. prepare the environment-friendly function material method for sewage disposal according to a kind of metallurgical slag reformation described in claim 1, wherein said acid includes organic acid (acetic acid, benzoic acid, heteropoly acid) and mineral acid (hydrochloric acid, nitric acid, sulphuric acid, sulfurous acid, phosphoric acid), and acid concentration is 2-6mol/L.
3. preparing the environment-friendly function material method for sewage disposal according to a kind of metallurgical slag reformation described in claim 1, wherein said acid solution and slag mass ratio are 10-40, and acid solubility temperature is 70-120 DEG C.
4. prepare the environment-friendly function material method for sewage disposal, wherein said PH=8-13 according to a kind of metallurgical slag reformation described in claim 1.
5. preparing the environment-friendly function material method for sewage disposal according to a kind of metallurgical slag reformation described in claim 1, wherein said hydrothermal synthesizing condition is 100-200 DEG C, 6-50h.
6. preparing the environment-friendly function material method for sewage disposal according to a kind of metallurgical slag reformation described in claim 1, wherein said baking temperature is 80-200 DEG C.
7. preparing the environment-friendly function material method for sewage disposal according to a kind of metallurgical slag reformation described in claim 1, wherein said powder is functional material houghite, its cation M3+For Fe3+、Al3+In one or both, M2+For Ca2+、Mg2+、Mn2+In one or more.
8. preparing the environment-friendly function material method for sewage disposal according to a kind of metallurgical slag reformation described in claim 1, wherein said cationic red initial concentration is 5-100ppm, adsorbent amount 0.5-4g/L, adsorption temp 20-65 DEG C, time 0.5-4h.
9. preparing the environment-friendly function material method for sewage disposal according to a kind of metallurgical slag reformation described in claim 1, wherein said Cr (VI) initial concentration is 3-100ppm, adsorbent amount 0.3-4g/L, adsorption temp 20-65 DEG C, time 0.3-6h.
10. prepare the environment-friendly function material method for sewage disposal, wherein said Cu according to a kind of metallurgical slag reformation described in claim 12+Initial concentration is 5-200ppm, adsorbent amount 0.6-6g/L, adsorption temp 20-80 DEG C, time 0.5-6h.
11. prepare the environment-friendly function material method for sewage disposal, wherein said VO according to a kind of metallurgical slag reformation described in claim 13 -Initial concentration is 5-300ppm, adsorbent amount 0.5-10g/L, adsorption temp 20-65 DEG C, time 0.5-20h.
12. prepare the environment-friendly function material method for sewage disposal, wherein said H according to a kind of metallurgical slag reformation described in claim 12PO4 -Initial concentration is 1-100ppm, adsorbent amount 0.5-5g/L, adsorption temp 20-65 DEG C, time 0.3-8h.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106629914A (en) * | 2016-12-27 | 2017-05-10 | 天津市环境保护科学研究院 | Method for remediating heavy metal polluted water in situ through osmotic response brick and application |
| CN107653574A (en) * | 2017-09-25 | 2018-02-02 | 山东大学 | Polyacid/polymer-based nanometer flexible fiber film and preparation method thereof and photoresponse be erasable and metal reduction in application |
| CN108295806A (en) * | 2017-12-06 | 2018-07-20 | 柳州市柳晶科技股份有限公司 | A kind of method and application preparing desulfuration adsorbent using Industrial Solid Waste |
| CN109012641A (en) * | 2018-08-29 | 2018-12-18 | 宝钢湛江钢铁有限公司 | A kind of preparation method of modified steel scoria heavy metal absorbent |
| CN109200991A (en) * | 2018-09-14 | 2019-01-15 | 太原理工大学 | A kind of preparation method and applications of red mud one-step synthesis magnetic adsorbent |
| CN109574084A (en) * | 2018-12-05 | 2019-04-05 | 上海宝田新型建材有限公司 | A kind of preparation method and applications of metallurgy base carbonate hydrotalcite |
| CN109821519A (en) * | 2018-12-05 | 2019-05-31 | 上海宝田新型建材有限公司 | A kind of preparation method and applications of metallurgy base nitrate anion hydrotalcite |
| CN110407885A (en) * | 2019-08-02 | 2019-11-05 | 北京科技大学 | A method of metal-organic framework material is prepared using metallurgical mine solid waste |
| CN112456638A (en) * | 2020-09-29 | 2021-03-09 | 江苏环保产业技术研究院股份公司 | Modified steel slag filler and preparation method and application thereof |
| WO2022257352A1 (en) * | 2021-06-07 | 2022-12-15 | 江苏科技大学 | Method for harmlessly treating hexavalent chromium ions by using metallurgical desulfurization slag |
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| CN106629914A (en) * | 2016-12-27 | 2017-05-10 | 天津市环境保护科学研究院 | Method for remediating heavy metal polluted water in situ through osmotic response brick and application |
| CN106629914B (en) * | 2016-12-27 | 2022-12-27 | 天津市环境保护科学研究院 | Method for in-situ remediation of heavy metal polluted water body by using permeable reactive bricks and application |
| CN107653574B (en) * | 2017-09-25 | 2019-08-27 | 山东大学 | Polyacid/polymer-based nanometer flexible fiber film and preparation method thereof and photoresponse be erasable and metal reduction in application |
| CN107653574A (en) * | 2017-09-25 | 2018-02-02 | 山东大学 | Polyacid/polymer-based nanometer flexible fiber film and preparation method thereof and photoresponse be erasable and metal reduction in application |
| CN108295806A (en) * | 2017-12-06 | 2018-07-20 | 柳州市柳晶科技股份有限公司 | A kind of method and application preparing desulfuration adsorbent using Industrial Solid Waste |
| CN108295806B (en) * | 2017-12-06 | 2019-11-15 | 柳晶（长春）环保科技有限公司 | A kind of method and application preparing desulfuration adsorbent using Industrial Solid Waste |
| CN109012641A (en) * | 2018-08-29 | 2018-12-18 | 宝钢湛江钢铁有限公司 | A kind of preparation method of modified steel scoria heavy metal absorbent |
| CN109200991A (en) * | 2018-09-14 | 2019-01-15 | 太原理工大学 | A kind of preparation method and applications of red mud one-step synthesis magnetic adsorbent |
| CN109821519A (en) * | 2018-12-05 | 2019-05-31 | 上海宝田新型建材有限公司 | A kind of preparation method and applications of metallurgy base nitrate anion hydrotalcite |
| CN109574084A (en) * | 2018-12-05 | 2019-04-05 | 上海宝田新型建材有限公司 | A kind of preparation method and applications of metallurgy base carbonate hydrotalcite |
| CN109574084B (en) * | 2018-12-05 | 2021-01-22 | 上海宝田新型建材有限公司 | Preparation method and application of metallurgical-base carbonate hydrotalcite |
| CN109821519B (en) * | 2018-12-05 | 2021-12-17 | 上海宝田新型建材有限公司 | Preparation method of metallurgical-based nitrate hydrotalcite |
| CN110407885A (en) * | 2019-08-02 | 2019-11-05 | 北京科技大学 | A method of metal-organic framework material is prepared using metallurgical mine solid waste |
| CN112456638A (en) * | 2020-09-29 | 2021-03-09 | 江苏环保产业技术研究院股份公司 | Modified steel slag filler and preparation method and application thereof |
| WO2022257352A1 (en) * | 2021-06-07 | 2022-12-15 | 江苏科技大学 | Method for harmlessly treating hexavalent chromium ions by using metallurgical desulfurization slag |
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Application publication date: 20160817 |