CN111790352B - Adsorbent capable of removing heavy metals in industrial wastewater and preparation method thereof - Google Patents

Adsorbent capable of removing heavy metals in industrial wastewater and preparation method thereof Download PDF

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CN111790352B
CN111790352B CN202010599508.3A CN202010599508A CN111790352B CN 111790352 B CN111790352 B CN 111790352B CN 202010599508 A CN202010599508 A CN 202010599508A CN 111790352 B CN111790352 B CN 111790352B
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adsorbent
steel slag
heavy metals
preparation
industrial wastewater
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CN111790352A (en
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吴雨波
栗海峰
罗翔
罗文君
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China University of Geosciences
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China University of Geosciences
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
    • B01J20/041—Oxides or hydroxides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • C—CHEMISTRY; METALLURGY
    • 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
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • C—CHEMISTRY; METALLURGY
    • 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
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48—Sorbents characterised by the starting material used for their preparation
    • B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48—Sorbents characterised by the starting material used for their preparation
    • B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
    • B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48—Sorbents characterised by the starting material used for their preparation
    • B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
    • B01J2220/4887—Residues, wastes, e.g. garbage, municipal or industrial sludges, compost, animal manure; fly-ashes
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C02F2101/20—Heavy metals or heavy metal compounds
    • C02F2101/22—Chromium or chromium compounds, e.g. chromates

Abstract

The invention belongs to the technical field of industrial wastewater treatment adsorbents, and particularly relates to an adsorbent capable of removing heavy metals in industrial wastewater and a preparation method thereof. The preparation method of the adsorbent comprises the steps of mixing and stirring 10-20 wt% of sodium hydroxide and 80-90 wt% of water glass until sodium hydroxide particles are completely dissolved to obtain an alkali activator; mixing 55-65 wt% of saw powder, 20-30 wt% of steel slag powder and 10-20 wt% of alkali activator, and grinding for 0.5-1 h to obtain mixed powder; pressing the mixed powder under the pressure of 100-150 MPa to obtain a steel slag sawdust geopolymer precursor; drying the geopolymer precursor at 50-80 ℃, and then preserving heat for 1-2.5 h at 600-850 ℃ under the protection of nitrogen to obtain a steel slag and sawdust carbon composite material; and washing the steel slag sawdust carbon composite material with deionized water until the pH value of washing water is 5-7 to obtain the adsorbent. The preparation method has the advantages of low cost, simple process, easy industrial production and the like, and the prepared easily-recycled adsorbent for removing heavy metals in industrial wastewater has good adsorption effect on the heavy metals and is easy to recycle.

Description

Adsorbent capable of removing heavy metals in industrial wastewater and preparation method thereof
Technical Field
The invention belongs to the technical field of industrial wastewater treatment adsorbents, and particularly relates to an adsorbent capable of removing heavy metals in industrial wastewater and a preparation method thereof.
Background
The development of the industrialization process increases the discharge amount of the wastewater containing heavy metal ions, pollutes water and soil, and directly influences the sanitary condition of drinking water of human beings. Therefore, the treatment of industrial wastewater containing heavy metal ions has become a focus of attention of world scholars. At present, methods for treating heavy metal ions in wastewater mainly include chemical precipitation, ion exchange, electrolysis, membrane separation, adsorption, and the like. The adsorption method is to adsorb one or more heavy metal ions in a water body by using an adsorbent and then achieve the purpose of separating and enriching heavy metals through desorption. The adsorption method has the advantages of high adsorption efficiency, wide material source and simple operation, and is generally concerned by people. Generally, the adsorbent is a key factor determining the adsorption efficiency and cost, and currently, the adsorbent most used in industry is activated carbon, and the adsorption capacity of the activated carbon on heavy metals is improved by modifying the activated carbon. For example, in the patent technology of 'a sewage treatment adsorbent and a preparation and use method thereof' (CN 109289780A), the modified corncob, the modified shaddock peel and the activated carbon are mixed, and the adsorption capacity of heavy metals is improved by a method of increasing the surface pores of the adsorbent. The patent technology of 'a preparation method of modified activated carbon for synchronously removing heavy metals and organic matters in sewage' (CN 108479698A) comprises the steps of pretreating activated carbon, soaking the pretreated activated carbon in potassium permanganate and hydrogen peroxide, soaking the soaked activated carbon in acetic acid and sodium acetate, drying, roasting the dried activated carbon in a nitrogen atmosphere at 500-600 ℃, soaking the roasted activated carbon in a sodium dodecyl sulfate solution, drying, roasting, and deeply activating the roasted activated carbon by using steam to prepare the activated carbon with heavy metal adsorption capacity. The adsorbent is complex in preparation process and high in price, and the powdery adsorbent is dispersed in liquid and is difficult to separate, difficult to recover and easy to cause secondary pollution.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of an adsorbent for removing heavy metals in industrial wastewater, which is low in cost, simple in preparation process and easy to recover.
The invention provides a preparation method of an adsorbent capable of removing heavy metals in industrial wastewater, which mainly comprises the following steps:
s1, mixing 10-20 wt% of sodium hydroxide and 80-90 wt% of water glass, and uniformly stirring until solid sodium hydroxide particles are completely dissolved to obtain an alkali activator;
s2, mixing 55-65 wt% of saw powder, 20-30 wt% of steel slag fine powder and 10-20 wt% of alkali activator, and grinding to obtain uniformly mixed powder;
s3, putting the mixed powder into a die, and performing high-pressure molding to obtain a steel slag sawdust geopolymer precursor;
s4, drying and roasting the geopolymer precursor in sequence, preserving heat, and cooling to obtain the steel slag sawdust carbon composite material;
s5, repeatedly washing the steel slag sawdust carbon composite material with deionized water until the pH value of washing water is 5-7, and obtaining the adsorbent.
Furthermore, the modulus of the water glass in S1 is 2.0-3.5.
Furthermore, the granularity of the steel slag fine powder in the S2 is less than or equal to 200 meshes.
Furthermore, the granularity of the saw powder in S2 is 500-200 meshes, and the wood content is more than or equal to 85 wt%.
Further, the grinding time in S2 is 0.5-1 h.
Further, the pressure condition of the high-pressure forming in S3 is 100-150 MPa, and the time is 1-3 min.
Further, the temperature condition of the drying treatment in the S4 is 50-80 ℃, the drying time is 8-12 h, the dried geopolymer precursor is roasted under the protection of nitrogen, and the roasting temperature condition is 600-850 ℃.
An adsorbent obtained by the above preparation method.
The application of the adsorbent is characterized in that the adsorption capacity of the adsorbent to heavy metal Cr (VI) ions in wastewater is 35.10-55.10 mg/g.
The technical scheme provided by the invention has the beneficial effects that: the preparation method of the adsorbent for removing heavy metals in industrial wastewater has the following advantages:
(1) according to the preparation method, the traditional industrial and agricultural wastes such as sawdust and metallurgical slag are used as raw materials, so that the cost is low, the wastes can be reasonably reused while the waste water is treated, and the effects of changing wastes into valuables and treating wastes with wastes are achieved;
(2) the preparation method of the invention takes the steel slag geopolymer as a framework, the saw dust activated carbon is filled in the framework, and the activated carbon is fixed in the pore canal of the steel slag geopolymer by adopting pressure forming to form the adsorbent with a staggered and compact unique structure, and the adsorbent is endowed with stable appearance, excellent mechanical property and excellent heavy metal ion adsorption capacity, thereby overcoming the defect that powdery activated carbon without fixed shape is difficult to recover after being adsorbed, avoiding secondary pollution to water resources, and having the advantages of simple solid-liquid separation and easy recovery;
(3) the preparation method does not need special equipment, has simple preparation process and is easy for industrial production;
(4) the adsorbent prepared by the method has a stable shape and a unique microstructure, and has the advantages of strong heavy metal adsorption capacity, simple separation and high recovery rate.
Drawings
FIG. 1 is a flow chart of a method for preparing an adsorbent for removing heavy metals from industrial wastewater according to the present invention;
FIG. 2 is an SEM image of an adsorbent according to the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be further described with reference to the accompanying drawings.
Referring to fig. 1, the present invention provides a method for preparing an adsorbent capable of removing heavy metals from industrial wastewater. The specific steps are shown in the following examples.
Here, the raw materials and instruments used in the following examples are commercially available. Wherein the sodium hydroxide is industrial-grade sodium hydroxide, and the NaOH content in the sodium hydroxide is more than or equal to 99.0 wt%; the granularity of the steel slag fine powder is less than or equal to 200 meshes; the granularity of the saw powder is 500-200 meshes, and the wood content is more than or equal to 85 wt%; the water glass is industrial water glass, and the modulus of the water glass is 2.0-3.5.
< example 1>
A preparation method of an adsorbent capable of removing heavy metals in industrial wastewater mainly comprises the following steps:
s1, mixing and stirring 10 wt% of sodium hydroxide and 90 wt% of water glass uniformly until solid sodium hydroxide particles are completely dissolved to obtain an alkali activator; wherein the modulus of the water glass is 2.2;
s2, mixing 58 wt% of saw powder, 28 wt% of steel slag fine powder and 14 wt% of alkali activator, and grinding for 0.5-1 h in a grinder to obtain uniformly mixed powder;
s3, placing the mixed powder into a mold, and keeping the mixed powder for 1-3 min under the pressure condition of 110MPa to obtain a steel slag sawdust geopolymer precursor;
s4, drying the geopolymer precursor in an oven at 50-65 ℃ for 8-10 hours, roasting at 600-750 ℃ under the protection of nitrogen, preserving heat for 1-2.5 hours, and cooling to obtain the steel slag sawdust carbon composite material;
s5, repeatedly washing the steel slag sawdust carbon composite material with deionized water for 3-5 times until the pH value of washing water is 5-7, and obtaining the adsorbent.
< example 2>
A preparation method of an adsorbent capable of removing heavy metals in industrial wastewater mainly comprises the following steps:
s1, mixing and stirring 15 wt% of sodium hydroxide and 85 wt% of water glass uniformly until solid sodium hydroxide particles are completely dissolved to obtain an alkali activator; wherein the modulus of the water glass is 2.8;
s2, mixing 60 wt% of saw powder, 25 wt% of steel slag fine powder and 15 wt% of alkali activator, and grinding for 0.5-1 h in a grinder to obtain uniformly mixed powder;
s3, placing the mixed powder into a mold, and keeping the mixed powder for 1-3 min under the pressure condition of 130MPa to obtain a steel slag sawdust geopolymer precursor;
s4, drying the geopolymer precursor in an oven at the temperature of 60-75 ℃ for 9-11 hours, roasting at the temperature of 700-800 ℃ under the protection of nitrogen, preserving heat for 1-2.5 hours, and cooling to obtain the steel slag sawdust carbon composite material;
s5, repeatedly washing the steel slag sawdust carbon composite material with deionized water for 3-5 times until the pH value of washing water is 5-7, and obtaining the adsorbent.
< example 3>
A preparation method of an adsorbent capable of removing heavy metals in industrial wastewater mainly comprises the following steps:
s1, mixing and stirring 20 wt% of sodium hydroxide and 80 wt% of water glass uniformly until solid sodium hydroxide particles are completely dissolved to obtain an alkali activator; wherein the modulus of the water glass is 3.4;
s2, mixing 62 wt% of saw powder, 22 wt% of steel slag fine powder and 16 wt% of alkali activator, and grinding for 0.5-1 h in a grinder to obtain uniformly mixed powder;
s3, placing the mixed powder into a mold, and keeping the mixed powder for 1-3 min under the pressure condition of 150MPa to obtain a steel slag sawdust geopolymer precursor;
s4, drying the geopolymer precursor in an oven at 70-80 ℃ for 18-12 h, roasting at 750-850 ℃ under the protection of nitrogen, preserving heat for 1-2.5 h, and cooling to obtain the steel slag sawdust carbon composite material;
s5, repeatedly washing the steel slag sawdust carbon composite material with deionized water for 3-5 times until the pH value of washing water is 5-7, and obtaining the adsorbent.
The compressive strength test is carried out on the adsorbents respectively prepared in the 3 embodiments of the invention, so that the compressive strength of the adsorbents in the 3 embodiments is 1.5-3.5 MPa. The specific surface areas of the adsorbents prepared in 3 examples were 127.53m2G, 132.73 and 143.91m2The total pore volume is 0.1235cm3G, 0.1241 and 0.1261cm3In terms of a/g, the average pore diameters were 10.46nm, 11.21 nm and 11.95nm, respectively. Further, the adsorption performance of the adsorbents of 3 examples was sequentially examined, and it was found that: when the pH value of the wastewater is 2-7, the adsorption quantity of the wastewater on heavy metal Cr (VI) ions in the wastewater is 35.10-55.10 mg/g; the adsorption capacity of the heavy metal Ce (III) ions in the wastewater is 277.34-352.81 mg/g.
The adsorbent prepared by the embodiments of the invention takes the steel slag geopolymer as a framework, the saw dust activated carbon is filled in the framework, and the activated carbon is fixed in the pore channels of the cylindrical steel slag geopolymer by pressure forming and has a staggered and compact unique structure. The adsorbent has stable appearance and excellent mechanical property, overcomes the defect that the powdery active carbon without fixed shape is difficult to recover after adsorption, avoids secondary pollution to water resources, and has the advantages of simple solid-liquid separation and easy recovery.
In this document, the terms front, back, upper and lower are used to define the components in the drawings and the positions of the components relative to each other, and are used for clarity and convenience of the technical solution. It is to be understood that the use of the directional terms should not be taken to limit the scope of the claims.
The features of the embodiments and embodiments described herein above may be combined with each other without conflict.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (6)

1. A preparation method of an adsorbent capable of removing heavy metals in industrial wastewater is characterized by mainly comprising the following steps:
s1, mixing 10-20 wt% of sodium hydroxide and 80-90 wt% of water glass, and uniformly stirring until sodium hydroxide solid particles are completely dissolved to obtain an alkali activator, wherein the modulus of the water glass is 2.0-3.5;
s2, mixing 55-65 wt% of saw powder, 20-30 wt% of steel slag fine powder and 10-20 wt% of alkali activator, and grinding to obtain uniformly mixed powder, wherein the granularity of the steel slag fine powder is less than or equal to 200 meshes, the granularity of the saw powder is 500-200 meshes, and the wood content is more than or equal to 85 wt%;
s3, putting the mixed powder into a die, and performing high-pressure molding to obtain a steel slag sawdust geopolymer precursor;
s4, drying and roasting the geopolymer precursor in sequence, preserving heat, and cooling to obtain the steel slag sawdust carbon composite material;
s5, repeatedly washing the steel slag sawdust carbon composite material with deionized water until the pH value of washing water is 5-7, and obtaining the adsorbent.
2. The preparation method of the adsorbent for removing heavy metals from industrial wastewater according to claim 1, wherein the grinding time in S2 is 0.5-1 h.
3. The method for preparing an adsorbent capable of removing heavy metals from industrial wastewater according to claim 1, wherein the pressure condition of the high-pressure forming in S3 is 100-150 MPa, and the time is 1-3 min.
4. The preparation method of the adsorbent for removing heavy metals from industrial wastewater according to claim 1, wherein the drying temperature in S4 is 50-80 ℃, the drying time is 8-12 h, the dried geopolymer precursor is roasted under the protection of nitrogen, and the roasting temperature is 600-850 ℃.
5. An adsorbent obtained by the production method according to any one of claims 1 to 4.
6. The application of the adsorbent according to claim 5, wherein the adsorption amount of the adsorbent to heavy metal Cr (VI) ions in wastewater is 35.10-55.10 mg/g.
CN202010599508.3A 2020-06-28 2020-06-28 Adsorbent capable of removing heavy metals in industrial wastewater and preparation method thereof Active CN111790352B (en)

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CN113426421B (en) * 2021-06-30 2022-07-22 深圳信息职业技术学院 Foamed geopolymer adsorption material and preparation method and application thereof
CN116173905A (en) * 2023-03-21 2023-05-30 西安建筑科技大学 Preparation and application of pyrolytic biochar/geopolymer composite material
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CN102698707A (en) * 2012-06-29 2012-10-03 武汉钢铁(集团)公司 Industrial wastewater adsorbent and preparation method thereof
CN102836697A (en) * 2012-09-04 2012-12-26 中国科学院唐山高新技术研究与转化中心 Stainless steel waste residue composite adsorbent and preparation method thereof
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CN110624498B (en) * 2018-06-21 2022-08-16 宝山钢铁股份有限公司 Composite steel slag-based heavy metal adsorbent
CN109012641B (en) * 2018-08-29 2021-07-13 宝钢湛江钢铁有限公司 Preparation method of modified steel slag heavy metal adsorbent
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