CN117696021A - Gangue modified heavy metal adsorbent and preparation method thereof - Google Patents
Gangue modified heavy metal adsorbent and preparation method thereof Download PDFInfo
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- 239000003463 adsorbent Substances 0.000 title claims abstract description 106
- 229910001385 heavy metal Inorganic materials 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000010902 straw Substances 0.000 claims abstract description 61
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims abstract description 25
- 241000209140 Triticum Species 0.000 claims abstract description 21
- 235000021307 Triticum Nutrition 0.000 claims abstract description 21
- 238000003756 stirring Methods 0.000 claims description 60
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 42
- 239000003245 coal Substances 0.000 claims description 41
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 38
- 238000005406 washing Methods 0.000 claims description 37
- 238000001914 filtration Methods 0.000 claims description 35
- 239000000843 powder Substances 0.000 claims description 34
- 229920002678 cellulose Polymers 0.000 claims description 32
- 239000001913 cellulose Substances 0.000 claims description 32
- 239000007788 liquid Substances 0.000 claims description 32
- 238000001035 drying Methods 0.000 claims description 31
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 26
- 239000006185 dispersion Substances 0.000 claims description 25
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 23
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 23
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 23
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 23
- 238000010438 heat treatment Methods 0.000 claims description 20
- 239000002253 acid Substances 0.000 claims description 17
- 238000002386 leaching Methods 0.000 claims description 17
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 15
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 11
- 239000002808 molecular sieve Substances 0.000 claims description 11
- 229910000077 silane Inorganic materials 0.000 claims description 11
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 11
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 10
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- 238000001354 calcination Methods 0.000 claims description 10
- 239000011812 mixed powder Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 239000002243 precursor Substances 0.000 claims description 10
- 238000007873 sieving Methods 0.000 claims description 10
- FOCAUTSVDIKZOP-UHFFFAOYSA-N chloroacetic acid Chemical compound OC(=O)CCl FOCAUTSVDIKZOP-UHFFFAOYSA-N 0.000 claims description 7
- 229940106681 chloroacetic acid Drugs 0.000 claims description 7
- 235000019441 ethanol Nutrition 0.000 claims description 7
- UKLNMMHNWFDKNT-UHFFFAOYSA-M sodium chlorite Chemical compound [Na+].[O-]Cl=O UKLNMMHNWFDKNT-UHFFFAOYSA-M 0.000 claims description 7
- 229960002218 sodium chlorite Drugs 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 6
- 239000000654 additive Substances 0.000 claims description 6
- 230000000996 additive effect Effects 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 239000005708 Sodium hypochlorite Substances 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000004108 freeze drying Methods 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 5
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 5
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 5
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 5
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 229940073455 tetraethylammonium hydroxide Drugs 0.000 claims description 5
- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-UHFFFAOYSA-M 0.000 claims description 5
- 238000001179 sorption measurement Methods 0.000 abstract description 61
- 230000000052 comparative effect Effects 0.000 description 30
- 239000010949 copper Substances 0.000 description 15
- 238000002474 experimental method Methods 0.000 description 15
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- 238000011069 regeneration method Methods 0.000 description 9
- 239000002699 waste material Substances 0.000 description 8
- 125000003172 aldehyde group Chemical group 0.000 description 6
- 230000001965 increasing effect Effects 0.000 description 6
- 125000003277 amino group Chemical group 0.000 description 5
- 238000003795 desorption Methods 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
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- 125000004122 cyclic group Chemical group 0.000 description 3
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- 241000196324 Embryophyta Species 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 125000000879 imine group Chemical group 0.000 description 2
- 239000010842 industrial wastewater Substances 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 241000282414 Homo sapiens Species 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 229910002800 Si–O–Al Inorganic materials 0.000 description 1
- 229910002808 Si–O–Si Inorganic materials 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
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- 230000006872 improvement Effects 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
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Abstract
The invention discloses a gangue modified heavy metal adsorbent and a preparation method thereof, and the gangue modified heavy metal adsorbent comprises the following components in parts by weight: 90-135 parts of gangue adsorbent, 10-16 parts of wheat straw and 3-5 parts of gamma-aminopropyl triethoxysilane. The invention provides a gangue modified heavy metal adsorbent and a preparation method thereof, and aims to solve the problems of low adsorption capacity and poor regenerability of the adsorbent.
Description
Technical Field
The invention belongs to the technical field of adsorbents, and particularly relates to a gangue modified heavy metal adsorbent and a preparation method thereof.
Background
The coal gangue is a rock which is obtained in the process of mining, separating and washing coal and is associated and symbiotic with coal, is industrial solid waste generated in the process of coal production and processing, has complex components, has different regional components, and has the main components of silicon dioxide and aluminum oxide in terms of chemical components; the large amount of coal gangue is piled up to occupy the land, collapse, spontaneous combustion and even explosion are easy to occur after piling, the coal gangue is easy to weather, dust can be generated when the coal gangue meets wind to cause atmospheric pollution, and in addition, the carried heavy metal elements penetrate underground along with rainwater to cause soil and water pollution and other problems, so that the effective utilization of the coal gangue is a problem to be solved urgently; cellulose is the most abundant polysaccharide substance on the earth, but a large amount of cellulose such as straw is only burned as waste, or is limited to be applied to low added value industry industries such as papermaking, so that great resource waste is caused, and serious environmental pollution can be even caused if the waste is not effectively treated; the main pollutants in the industrial wastewater are heavy metals such as lead, cadmium, iron, copper, zinc, mercury, silver and the like in the form of ions or hydrates, the heavy metals are difficult to naturally degrade and easily gather, metal oxides with severe toxicity are easy to generate, if the industrial wastewater is not treated and directly discharged, heavy metal pollution of large soil and water sources can be caused, the growth environment of plants in the ground and water and the ecological structure of the region are damaged, and the enrichment of the heavy metals in animals and plants finally endangers the life and health of human beings along with food chains; the adsorption method for treating sewage by using the adsorbent is widely used because of the advantages of simple operation, recoverable heavy metals and the like, and adsorption can be divided into physical adsorption, chemical adsorption and ion exchange adsorption according to the action mode between the adsorbent and pollutants, but the existing adsorption materials such as active carbon, organic resin, molecular sieve and the like have the problems of high regeneration cost, limited adsorption capacity, poor reproducibility and the like and are limited in use.
The prior art mainly has the following problems: the adsorption capacity of the adsorbent prepared from the gangue is low, and the regeneration cost is high.
Disclosure of Invention
Aiming at the situation, in order to overcome the defects of the prior art, the invention provides the gangue modified heavy metal adsorbent and the preparation method thereof, and in order to solve the problems of low adsorption quantity and poor regenerability of the adsorbent, the invention provides the preparation of the gangue adsorbent by means of alkali hot melting and acid leaching, so that the high specific surface area of the gangue adsorbent is realized, the modified cellulose is prepared by straw, the gangue adsorbent treated by the silane coupling agent is modified, the specific surface area is increased, the active groups are increased, and the improvement of the adsorption effect of the adsorbent on heavy metals is realized.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: the invention provides a gangue modified heavy metal adsorbent and a preparation method thereof, wherein the gangue modified heavy metal adsorbent comprises the following components in parts by weight: 90-135 parts of gangue adsorbent, 10-16 parts of wheat straw and 3-5 parts of gamma-aminopropyl triethoxysilane.
Preferably, the preparation method of the gangue adsorbent specifically comprises the following steps:
step one, crushing and grinding the coal gangue, sieving the crushed coal gangue with a 200-mesh sieve to obtain coal gangue powder, and uniformly mixing sodium carbonate and the coal gangue powder in a mass ratio of 0.5-0.7:1 to obtain mixed powder;
step two, adding the mixed powder obtained in the step one into a muffle furnace, calcining for 5 hours at the temperature of 800 ℃ to obtain a calcined product, adding the calcined product into sulfuric acid solution with the molar concentration of 4mol/L for acid leaching according to the addition amount of 0.08-0.12g/mL, carrying out heat preservation and stirring for 4-6 hours at the temperature of 85-95 ℃, filtering, washing and drying to obtain an acid leaching product;
step three, adding the acid leaching product obtained in the step two into sodium bicarbonate solution with the mass concentration of 0.4% by adding the additive amount of 0.12-0.16g/mL, stirring to obtain a dispersion liquid, dripping tetraethylammonium hydroxide into the dispersion liquid by adding the additive amount of 0.15-0.17g/mL, heating and stirring at 90 ℃ for 1h to obtain a mixed liquid, adding polyaluminium chloride into the mixed liquid by adding the additive amount of 0.8-1.2g/mL, uniformly mixing, heating and stirring at 90 ℃ for 5h to obtain a molecular sieve precursor;
and step four, adding the molecular sieve precursor obtained in the step three into a hydrothermal kettle, heating at 180 ℃ for reaction for 48 hours, filtering, washing, drying, cooling to room temperature, heating to 600 ℃ at a speed of 5 ℃/min, and continuously calcining for 2 hours at 600 ℃ to obtain the coal gangue adsorbent.
Preferably, the preparation method of the gangue modified heavy metal adsorbent specifically comprises the following steps:
s1, adding a gangue adsorbent into a gamma-aminopropyl triethoxysilane solution with the volume concentration of 3.5% by taking absolute ethyl alcohol as a solvent, stirring in a water bath at 60 ℃ for 6 hours, filtering, washing and drying to obtain a silane modified adsorbent;
s2, cleaning, airing, drying and crushing the wheat straw, sieving with a 50-mesh sieve to obtain straw powder, adding the straw powder into 5% sodium hydroxide solution, carrying out water bath at 80 ℃ for 2 hours, and filtering and washing to obtain alkalized straw powder;
s3, adding the alkalized straw powder obtained in the step S2 into a sodium chlorite solution with the molar concentration of 25mol/L, adjusting the pH value to 6-7, stirring in a 75 ℃ water bath for 40min, filtering, washing and drying to obtain straw cellulose;
s4, adding the straw cellulose obtained in the step S3 into an 80% ethanol solution, stirring in a water bath at 65 ℃ for 30min to obtain cellulose dispersion liquid, adding sodium hydroxide, continuing to keep the temperature and stir for 2h, then adding chloroacetic acid, continuing to keep the temperature and stir for 1.5h, adjusting the pH value to 6, and filtering and washing to obtain carboxymethyl cellulose;
s5, adding the carboxymethyl cellulose obtained in the step S4 into deionized water, uniformly stirring, adding sodium hypochlorite with the molar quantity of 1.5-2.5 times, uniformly stirring, carrying out light-shielding reaction for 2-3 hours, adding ethylene glycol to terminate the reaction, dialyzing, concentrating, and freeze-drying to obtain oxidized carboxymethyl cellulose;
s6, adding the silane modified adsorbent obtained in the step S1 into water, adding the oxidized carboxymethyl cellulose obtained in the step S5, stirring in a water bath for 20 hours, filtering, washing and drying to obtain the gangue modified heavy metal adsorbent.
Preferably, in S1, the addition amount of the gangue adsorbent in the gamma-aminopropyl triethoxysilane solution is 40-60mg/mL;
preferably, in S2, the addition amount of the straw powder in the sodium hydroxide solution is 50-55mg/mL;
preferably, in S3, the addition amount of the alkalized straw powder in the sodium chlorite solution is 0.08-0.12g/mL;
preferably, in S4, the addition amount of the straw cellulose in the ethanol solution is 0.13-0.15g/mL;
preferably, in S4, the addition amount of the sodium hydroxide is 6-9% of the mass percentage of the cellulose dispersion;
preferably, in S4, the chloroacetic acid is added in an amount of 7-8% by mass of the cellulose dispersion.
The beneficial effects obtained by the invention are as follows: the method comprises the steps of processing coal gangue in an alkali hot melting and acid leaching mode, wherein the main components of the coal gangue are silicon dioxide and aluminum oxide, a large amount of Si-O-Si and Al-O-Al bonds can generate the adsorption effect of dipole-dipole bonds, polyaluminium chloride is added to further adjust the silicon-aluminum ratio, so that the coal gangue adsorbent with a porous structure is prepared, the pore diameter of micropores is widened, the specific surface area is increased, gamma-aminopropyl triethoxysilane is used for carrying out surface functionalization modification on the coal gangue adsorbent, amino groups are loaded on the surface and in the pore structure of the coal gangue, the adsorption capacity of heavy metal cations is enhanced through the chemical adsorption effect of functional groups, cellulose is prepared from wheat straw, carboxymethylation and oxidation modification are carried out, carboxymethyl cellulose with carboxymethyl and aldehyde groups is obtained, the aldehyde groups of the carboxymethyl cellulose are combined with amino groups on the silane modified adsorbent to obtain a stable cross-linked structure, the coal gangue adsorbent is uniformly loaded on the coal gangue, the specific surface area of the adsorbent and the loading capacity of the aldehyde groups and the carboxymethyl groups are increased, the adsorption effect of the adsorbent on heavy metal ions is further improved, the aldehyde groups and the amino groups form an imine structure which can be used as an adsorbent to form an electronic complex with the heavy metal ion, and the adsorption effect is improved; in addition, the gangue and the straw are common wastes in life production, and the adsorbent prepared by using the gangue and the straw as raw materials is applied to the aspects of industrial sewage and the like, so that the effects of waste utilization and waste treatment by waste are achieved, the environment is protected, and a new way is provided for the effective utilization of the wastes.
Drawings
FIG. 1 is a graph showing the results of adsorption experiments of the present invention for examples 1 to 3 and comparative examples 1 to 3Cr (VI);
FIG. 2 is a graph showing the results of the Cu (II) adsorption experiments of examples 1 to 3 and comparative examples 1 to 3 of the present invention;
FIG. 3 is a graph showing the results of adsorption experiments of Pb (II) in examples 1 to 3 and comparative examples 1 to 3 of the present invention;
FIG. 4 is a graph showing the results of cyclic desorption experiments of examples 1 to 3 and comparative example 2 according to the present invention.
The accompanying drawings are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate the invention and together with the embodiments of the invention, serve to explain the invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention; all other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. In addition, any methods and materials similar or equivalent to those described herein can be used in the present invention. The preferred methods and materials described herein are illustrative only and should not be construed as limiting the scope of the present application.
The experimental methods in the following examples are all conventional methods unless otherwise specified; the test materials and test strains used in the examples described below, unless otherwise specified, were commercially available.
Example 1
The gangue modified heavy metal adsorbent comprises the following components in parts by weight: 90 parts of gangue adsorbent, 10 parts of wheat straw and 3 parts of gamma-aminopropyl triethoxysilane.
The preparation method of the gangue adsorbent specifically comprises the following steps:
step one, crushing and grinding the coal gangue, sieving the crushed coal gangue with a 200-mesh sieve to obtain coal gangue powder, and uniformly mixing sodium carbonate and the coal gangue powder in a mass ratio of 0.5:1 to obtain mixed powder;
step two, adding the mixed powder obtained in the step one into a muffle furnace, calcining for 5 hours at the temperature of 800 ℃ to obtain a calcined product, adding the calcined product into a sulfuric acid solution with the molar concentration of 4mol/L for acid leaching according to the addition amount of 0.08g/mL, carrying out heat preservation and stirring for 4 hours at the temperature of 85 ℃, filtering, washing and drying to obtain an acid leaching product;
step three, adding the acid leaching product obtained in the step two into sodium bicarbonate solution with the mass concentration of 0.4% according to the addition amount of 0.12g/mL, stirring to obtain dispersion liquid, dripping tetraethylammonium hydroxide into the dispersion liquid according to the addition amount of 0.15g/mL, heating and stirring at 90 ℃ for 1h to obtain mixed liquid, adding polyaluminium chloride into the mixed liquid according to the addition amount of 0.8g/mL, uniformly mixing, and heating and stirring at 90 ℃ for 5h to obtain a molecular sieve precursor;
and step four, adding the molecular sieve precursor obtained in the step three into a hydrothermal kettle, heating at 180 ℃ for reaction for 48 hours, filtering, washing, drying, cooling to room temperature, transferring into a muffle furnace, heating to 600 ℃ at a speed of 5 ℃/min, and continuously calcining for 2 hours at 600 ℃ to obtain the coal gangue adsorbent.
The preparation method of the gangue modified heavy metal adsorbent specifically comprises the following steps:
s1, adding a gangue adsorbent into a gamma-aminopropyl triethoxysilane solution with the volume concentration of 3.5% taking absolute ethyl alcohol as a solvent according to the addition amount of 40mg/mL, stirring in a water bath at 60 ℃ for 6 hours, filtering, washing and drying to obtain a silane modified adsorbent;
s2, cleaning, airing, drying and crushing the wheat straw, sieving with a 50-mesh sieve to obtain straw powder, adding the straw powder into a 5% sodium hydroxide solution according to the addition amount of 50mg/ml, carrying out water bath at 80 ℃ for 2 hours, and filtering and washing to obtain alkalized straw powder;
s3, adding the alkalized straw powder obtained in the step S2 into a sodium chlorite solution with the molar concentration of 25mol/L according to the addition amount of 0.08g/mL, adjusting the pH value to 6, stirring in a 75 ℃ water bath for 40min, filtering, washing and drying to obtain straw cellulose;
s4, adding the straw cellulose obtained in the S3 into an 80% ethanol solution, stirring in a water bath at 65 ℃ for 30min to obtain cellulose dispersion liquid, adding sodium hydroxide with the mass percentage of 6% of the cellulose dispersion liquid, continuously preserving heat and stirring for 2h, then adding chloroacetic acid with the mass percentage of 7% of the cellulose dispersion liquid, continuously preserving heat and stirring for 1.5h, adjusting the pH value to 6, and filtering and washing to obtain carboxymethyl cellulose;
s5, adding the carboxymethyl cellulose obtained in the step S4 into deionized water, uniformly stirring, adding sodium hypochlorite with the molar quantity of 1.5 times, uniformly stirring, carrying out light-shielding reaction for 2 hours, adding ethylene glycol to terminate the reaction, dialyzing, concentrating, and freeze-drying to obtain oxidized carboxymethyl cellulose;
s6, adding the silane modified adsorbent obtained in the step S1 into water, adding the oxidized carboxymethyl cellulose obtained in the step S5, stirring in a water bath for 20 hours, filtering, washing and drying to obtain the gangue modified heavy metal adsorbent.
Example 2
The gangue modified heavy metal adsorbent comprises the following components in parts by weight: 135 parts of gangue adsorbent, 16 parts of wheat straw and 5 parts of gamma-aminopropyl triethoxysilane.
The preparation method of the gangue adsorbent specifically comprises the following steps:
step one, crushing and grinding the coal gangue, sieving the crushed coal gangue with a 200-mesh sieve to obtain coal gangue powder, and uniformly mixing sodium carbonate and the coal gangue powder in a mass ratio of 0.7:1 to obtain mixed powder;
step two, adding the mixed powder obtained in the step one into a muffle furnace, calcining for 5 hours at the temperature of 800 ℃ to obtain a calcined product, adding the calcined product into a sulfuric acid solution with the molar concentration of 4mol/L for acid leaching in an adding amount of 0.12g/mL, carrying out heat preservation and stirring for 6 hours at the temperature of 95 ℃, filtering, washing and drying to obtain an acid leaching product;
step three, adding the acid leaching product obtained in the step two into sodium bicarbonate solution with the mass concentration of 0.4% according to the addition amount of 0.16g/mL, stirring to obtain dispersion liquid, dripping tetraethylammonium hydroxide into the dispersion liquid according to the addition amount of 0.17g/mL, heating and stirring at 90 ℃ for 1h to obtain mixed liquid, adding polyaluminium chloride into the mixed liquid according to the addition amount of 1.2g/mL, uniformly mixing, and heating and stirring at 90 ℃ for 5h to obtain a molecular sieve precursor;
and step four, adding the molecular sieve precursor obtained in the step three into a hydrothermal kettle, heating at 180 ℃ for reaction for 48 hours, filtering, washing, drying, cooling to room temperature, transferring into a muffle furnace, heating to 600 ℃ at a speed of 5 ℃/min, and continuously calcining for 2 hours at 600 ℃ to obtain the coal gangue adsorbent.
The preparation method of the gangue modified heavy metal adsorbent specifically comprises the following steps:
s1, adding a gangue adsorbent into a gamma-aminopropyl triethoxysilane solution with the volume concentration of 3.5% taking absolute ethyl alcohol as a solvent according to the addition amount of 60mg/mL, stirring in a water bath at 60 ℃ for 6 hours, filtering, washing and drying to obtain a silane modified adsorbent;
s2, cleaning, airing, drying and crushing the wheat straw, sieving with a 50-mesh sieve to obtain straw powder, adding the straw powder into 5% sodium hydroxide solution according to the adding amount of 55mg/ml, carrying out water bath at 80 ℃ for 2 hours, and filtering and washing to obtain alkalized straw powder;
s3, adding the alkalized straw powder obtained in the step S2 into a sodium chlorite solution with the molar concentration of 25mol/L according to the addition amount of 0.12g/mL, adjusting the pH value to 7, stirring in a 75 ℃ water bath for 40min, filtering, washing and drying to obtain straw cellulose;
s4, adding the straw cellulose obtained in the S3 into an 80% ethanol solution, stirring in a water bath at 65 ℃ for 30min to obtain cellulose dispersion liquid, adding sodium hydroxide with the mass percentage of 6-9% of the cellulose dispersion liquid, continuously preserving heat and stirring for 2h, then adding chloroacetic acid with the mass percentage of 7-8% of the cellulose dispersion liquid, continuously preserving heat and stirring for 1.5h, adjusting the pH value to 6, and filtering and washing to obtain carboxymethyl cellulose;
s5, adding the carboxymethyl cellulose obtained in the step S4 into deionized water, uniformly stirring, adding sodium hypochlorite with the molar quantity being 2.5 times, uniformly stirring, carrying out light-shielding reaction for 3 hours, adding ethylene glycol to terminate the reaction, dialyzing, concentrating, and freeze-drying to obtain oxidized carboxymethyl cellulose;
s6, adding the silane modified adsorbent obtained in the step S1 into water, adding the oxidized carboxymethyl cellulose obtained in the step S5, stirring in a water bath for 20 hours, filtering, washing and drying to obtain the gangue modified heavy metal adsorbent.
Example 3
The gangue modified heavy metal adsorbent comprises the following components in parts by weight: 100 parts of gangue adsorbent, 13 parts of wheat straw and 4 parts of gamma-aminopropyl triethoxysilane.
The preparation method of the gangue adsorbent specifically comprises the following steps:
step one, crushing and grinding the coal gangue, sieving the crushed coal gangue with a 200-mesh sieve to obtain coal gangue powder, and uniformly mixing sodium carbonate and the coal gangue powder in a mass ratio of 0.6:1 to obtain mixed powder;
step two, adding the mixed powder obtained in the step one into a muffle furnace, calcining for 5 hours at the temperature of 800 ℃ to obtain a calcined product, adding the calcined product into a sulfuric acid solution with the molar concentration of 4mol/L for acid leaching according to the addition amount of 0.09g/mL, carrying out heat preservation and stirring for 5 hours at the temperature of 90 ℃, filtering, washing and drying to obtain an acid leaching product;
step three, adding the acid leaching product obtained in the step two into sodium bicarbonate solution with the mass concentration of 0.4% according to the addition amount of 0.14g/mL, stirring to obtain a dispersion liquid, dripping tetraethylammonium hydroxide into the dispersion liquid according to the addition amount of 0.16g/mL, heating and stirring at 90 ℃ for 1h to obtain a mixed liquid, adding polyaluminium chloride into the mixed liquid according to the addition amount of 1g/mL, uniformly mixing, and heating and stirring at 90 ℃ for 5h to obtain a molecular sieve precursor;
and step four, adding the molecular sieve precursor obtained in the step three into a hydrothermal kettle, heating at 180 ℃ for reaction for 48 hours, filtering, washing, drying, cooling to room temperature, transferring into a muffle furnace, heating to 600 ℃ at a speed of 5 ℃/min, and continuously calcining for 2 hours at 600 ℃ to obtain the coal gangue adsorbent.
The preparation method of the gangue modified heavy metal adsorbent specifically comprises the following steps:
s1, adding a gangue adsorbent into a gamma-aminopropyl triethoxysilane solution with the volume concentration of 3.5% taking absolute ethyl alcohol as a solvent according to the addition amount of 50mg/mL, stirring in a water bath at 60 ℃ for 6 hours, filtering, washing and drying to obtain a silane modified adsorbent;
s2, cleaning, airing, drying and crushing the wheat straw, sieving with a 50-mesh sieve to obtain straw powder, adding the straw powder into a 5% sodium hydroxide solution according to the adding amount of 53mg/ml, carrying out water bath at 80 ℃ for 2 hours, and filtering and washing to obtain alkalized straw powder;
s3, adding the alkalized straw powder obtained in the step S2 into a sodium chlorite solution with the molar concentration of 25mol/L according to the addition amount of 0.1g/mL, adjusting the pH value to 6.5, stirring in a water bath at the temperature of 75 ℃ for 40min, filtering, washing and drying to obtain straw cellulose;
s4, adding the straw cellulose obtained in the S3 into an 80% ethanol solution, stirring in a water bath at 65 ℃ for 30min to obtain cellulose dispersion liquid, adding sodium hydroxide with the mass percentage of 7% of the cellulose dispersion liquid, continuously preserving heat and stirring for 2h, then adding chloroacetic acid with the mass percentage of 7.5% of the cellulose dispersion liquid, continuously preserving heat and stirring for 1.5h, adjusting the pH value to 6, and filtering and washing to obtain carboxymethyl cellulose;
s5, adding the carboxymethyl cellulose obtained in the step S4 into deionized water, uniformly stirring, adding sodium hypochlorite with the molar quantity being 2 times, uniformly stirring, carrying out light-shielding reaction for 2.5 hours, adding ethylene glycol to terminate the reaction, dialyzing, concentrating, and freeze-drying to obtain oxidized carboxymethyl cellulose;
s6, adding the silane modified adsorbent obtained in the step S1 into water, adding the oxidized carboxymethyl cellulose obtained in the step S5, stirring in a water bath for 20 hours, filtering, washing and drying to obtain the gangue modified heavy metal adsorbent.
Comparative example 1
This comparative example provides an adsorbent differing from example 1 only in that no wheat straw is contained in the components, and the remaining components, component contents, are the same as example 1.
Comparative example 2
This comparative example provides an adsorbent differing from example 1 only in that no gamma-aminopropyl triethoxysilane is included in the components, the remaining components, component contents being the same as in example 1.
Comparative example 3
This comparative example provides an adsorbent differing from example 1 only in that the components do not include wheat straw and gamma-aminopropyl triethoxysilane, and the remaining components and component contents are the same as in example 1.
Experimental example
Cr (VI) adsorption experiments
1g of the adsorbents obtained in examples 1 to 3 and comparative examples 1 to 3 were dried at 50℃and then added to 100mL of a solution of Cr (VI) having a concentration of 30mg/L, respectively, stirred at 300rpm for 100 minutes, centrifuged at 6000rpm for 3 minutes, and the concentration of Cr (VI) in the solution was measured by spectrophotometry, and the adsorption amount was calculated by the following formula:
cr (VI) adsorption amount= (initial Cr (VI) concentration-final Cr (VI) concentration) ×cr (VI) solution volume/adsorbent mass.
FIG. 1 is a graph showing the results of adsorption experiments of Cr (VI) in examples 1-3 and comparative examples 1-3 of the present invention, wherein the adsorption amounts of Cr (VI) in examples 1-3 and comparative examples 1-3 were 9.33mg/g, 9.26mg/g, 9.61mg/g, 6.93mg/g, 7.22mg/g, and 6.36mg/g, respectively; the adsorption amount of Cr (VI) in examples 1-3 is obviously higher than that in comparative example 1, which shows that the use of wheat straw improves the adsorption amount of Cr (VI) by the adsorbent, the adsorption amount of Cr (VI) in examples 1-3 is obviously higher than that in comparative example 2, the use of gamma-aminopropyl triethoxysilane improves the adsorption amount of Cr (VI) by the adsorbent, and the adsorption amount of Cr (VI) in examples 1-3 is obviously higher than that in comparative example 3, which shows that the use of both wheat straw and gamma-aminopropyl triethoxysilane improves the adsorption amount of Cr (VI) by the adsorbent. The gamma-aminopropyl triethoxy silane is used for carrying out surface functionalization modification on the gangue adsorbent, increasing amino groups, enhancing the adsorption capacity of heavy metal cations, preparing oxidized carboxymethyl cellulose from the wheat straw, carrying carboxymethyl and aldehyde groups, forming an imine structure with the amino groups as electron donors, improving the adsorption effect of the adsorbent on the heavy metal ions, and increasing the specific surface area of the adsorbent and the loading capacity of the aldehyde groups and the carboxymethyl groups, thereby improving the adsorption effect of the adsorbent on the heavy metal ions.
Cu (II) adsorption experiments
1g of the adsorbents obtained in examples 1 to 3 and comparative examples 1 to 3 were dried at 50℃and then added to 200mL of a Cu (II) solution having a concentration of 80mg/L, respectively, stirred at 300rpm for 100 minutes, centrifuged at 6000rpm for 3 minutes, and the concentration of Cu (II) in the solution was measured by spectrophotometry, and the adsorption amount was calculated by the following formula:
cu (ii) adsorption = (initial Cu (ii) concentration-final Cu (ii) concentration) ×cu (ii) solution volume/adsorbent mass.
FIG. 2 is a graph showing the results of the adsorption experiments of Cu (II) in examples 1 to 3 and comparative examples 1 to 3 of the present invention, wherein the adsorption amounts of Cu (II) in examples 1 to 3 and comparative examples 1 to 3 were 102.2mg/g, 96.9mg/g, 103.5mg/g, 82.6mg/g, 88.3mg/g, 75.1mg/g, respectively; the adsorption capacity of examples 1-3 on Cu (II) is obviously higher than that of comparative example 1, which shows that the use of wheat straw improves the adsorption capacity of the adsorbent on Cu (II), the adsorption capacity of examples 1-3 on Cu (II) is obviously higher than that of comparative example 2, the use of gamma-aminopropyl triethoxysilane improves the adsorption capacity of the adsorbent on Cu (II), and the adsorption capacity of examples 1-3 on Cu (II) is obviously higher than that of comparative example 3, which shows that the use of wheat straw and gamma-aminopropyl triethoxysilane together improves the adsorption capacity of the adsorbent on Cu (II).
Pb (II) adsorption experiments
1g of the adsorbents obtained in examples 1 to 3 and comparative examples 1 to 3 were dried at 50℃and then added to 200mL of a 100mg/L Pb (II) solution, respectively, stirred at 300rpm for 100 minutes, centrifuged at 6000rpm for 3 minutes, and the concentration of Pb (II) in the solution was measured by spectrophotometry, and the adsorption amount was calculated by the following formula:
pb (ii) adsorption amount= (Pb (ii) initial concentration-Pb (ii) final concentration) ×pb (ii) solution volume/adsorbent mass×100%.
FIG. 3 is a graph showing the results of adsorption experiments of Pb (II) in examples 1 to 3 and comparative examples 1 to 3 of the present invention, wherein the adsorption amounts of Pb (II) in examples 1 to 3 and comparative examples 1 to 3 were 122.6mg/g, 127.1mg/g, 119.3mg/g, 92.3mg/g, 89.5mg/g, 83.7mg/g, respectively; the adsorption capacity of Pb (II) in examples 1-3 is obviously higher than that in comparative example 1, which shows that the adsorption capacity of Pb (II) by the adsorbent is improved by the use of wheat straw, the adsorption capacity of Pb (II) in examples 1-3 is obviously higher than that in comparative example 2, the adsorption capacity of Pb (II) by the adsorbent is improved by the use of gamma-aminopropyl triethoxysilane, the adsorption capacity of Pb (II) in examples 1-3 is obviously higher than that in comparative example 3, and the adsorption capacity of Pb (II) by the adsorbent is improved by the use of the wheat straw and the gamma-aminopropyl triethoxysilane together.
4. Desorption experiment
Putting the adsorbed examples 1-3 into 0.1mol/L HCl solution to desorb for 1h, repeatedly washing the solution with deionized water until the solution is neutral, drying, carrying out Pb (II) adsorption experiments again, calculating the adsorption amount, carrying out 7 times, and calculating the regeneration rate according to the following formula:
regeneration rate=nth adsorption amount/1 st adsorption amount×100%.
FIG. 4 is a graph showing the results of cyclic desorption experiments of examples 1 to 3 and comparative example 2 according to the present invention, wherein the removal capacity of Pb (II) of the adsorbent tends to decrease with the increase of the number of experiments, and the regeneration rates of examples 1 to 3 and comparative example 2 are 86.3%, 86.5%, 86.1% and 71.6% respectively after 7 cyclic desorption; the Pb (II) adsorption capacity of examples 1-3 is still kept above 85%, which shows that the obtained adsorbent can be reused for many times, has good regeneration capacity, and the regeneration rate of examples 1-3 is higher than that of example 2, which shows that the use of gamma-aminopropyl triethoxysilane improves the regeneration rate of the material; the gamma-aminopropyl triethoxy silane tightly connects cellulose to coal gangue, reduces loss in the adsorption and desorption processes, and further improves the regeneration effect of the obtained adsorbent.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
The invention and its embodiments have been described above with no limitation, and the invention is illustrated in the figures of the accompanying drawings as one of its embodiments, without limitation in practice. In summary, those skilled in the art, having benefit of this disclosure, will appreciate that the invention can be practiced without the specific details disclosed herein.
Claims (8)
1. A gangue modified heavy metal adsorbent is characterized in that: the gangue modified heavy metal adsorbent comprises the following components in parts by weight: 90-135 parts of gangue adsorbent, 10-16 parts of wheat straw and 3-5 parts of gamma-aminopropyl triethoxysilane; the preparation method of the gangue adsorbent specifically comprises the following steps:
step one, crushing and grinding the coal gangue, sieving the crushed coal gangue with a 200-mesh sieve to obtain coal gangue powder, and uniformly mixing sodium carbonate and the coal gangue powder in a mass ratio of 0.5-0.7:1 to obtain mixed powder;
step two, adding the mixed powder obtained in the step one into a muffle furnace, calcining for 5 hours at the temperature of 800 ℃ to obtain a calcined product, adding the calcined product into sulfuric acid solution with the molar concentration of 4mol/L for acid leaching according to the addition amount of 0.08-0.12g/mL, carrying out heat preservation and stirring for 4-6 hours at the temperature of 85-95 ℃, filtering, washing and drying to obtain an acid leaching product;
step three, adding the acid leaching product obtained in the step two into sodium bicarbonate solution with the mass concentration of 0.4% by adding the additive amount of 0.12-0.16g/mL, stirring to obtain a dispersion liquid, dripping tetraethylammonium hydroxide into the dispersion liquid by adding the additive amount of 0.15-0.17g/mL, heating and stirring at 90 ℃ for 1h to obtain a mixed liquid, adding polyaluminium chloride into the mixed liquid by adding the additive amount of 0.8-1.2g/mL, uniformly mixing, heating and stirring at 90 ℃ for 5h to obtain a molecular sieve precursor;
and step four, adding the molecular sieve precursor obtained in the step three into a hydrothermal kettle, heating at 180 ℃ for reaction for 48 hours, filtering, washing, drying, cooling to room temperature, transferring into a muffle furnace, heating to 600 ℃ at a speed of 5 ℃/min, and continuously calcining for 2 hours at 600 ℃ to obtain the coal gangue adsorbent.
2. A method for preparing the gangue modified heavy metal adsorbent as claimed in claim 1, wherein: the method specifically comprises the following steps:
s1, adding a gangue adsorbent into a gamma-aminopropyl triethoxysilane solution with the volume concentration of 3.5% by taking absolute ethyl alcohol as a solvent, stirring in a water bath at 60 ℃ for 6 hours, filtering, washing and drying to obtain a silane modified adsorbent;
s2, cleaning, airing, drying and crushing the wheat straw, sieving with a 50-mesh sieve to obtain straw powder, adding the straw powder into 5% sodium hydroxide solution, carrying out water bath at 80 ℃ for 2 hours, and filtering and washing to obtain alkalized straw powder;
s3, adding the alkalized straw powder obtained in the step S2 into a sodium chlorite solution with the molar concentration of 25mol/L, adjusting the pH value to 6-7, stirring in a 75 ℃ water bath for 40min, filtering, washing and drying to obtain straw cellulose;
s4, adding the straw cellulose obtained in the step S3 into an 80% ethanol solution, stirring in a water bath at 65 ℃ for 30min to obtain cellulose dispersion liquid, adding sodium hydroxide, continuing to keep the temperature and stir for 2h, then adding chloroacetic acid, continuing to keep the temperature and stir for 1.5h, adjusting the pH value to 6, and filtering and washing to obtain carboxymethyl cellulose;
s5, adding the carboxymethyl cellulose obtained in the step S4 into deionized water, uniformly stirring, adding sodium hypochlorite with the molar quantity of 1.5-2.5 times, uniformly stirring, carrying out light-shielding reaction for 2-3 hours, adding ethylene glycol to terminate the reaction, dialyzing, concentrating, and freeze-drying to obtain oxidized carboxymethyl cellulose;
s6, adding the silane modified adsorbent obtained in the step S1 into water, adding the oxidized carboxymethyl cellulose obtained in the step S5, stirring in a water bath for 20 hours, filtering, washing and drying to obtain the gangue modified heavy metal adsorbent.
3. The method for preparing the gangue modified heavy metal adsorbent as claimed in claim 2, wherein: in S1, the addition amount of the gangue adsorbent in the gamma-aminopropyl triethoxysilane solution is 40-60mg/mL.
4. The method for preparing the gangue modified heavy metal adsorbent as claimed in claim 3, wherein: in S2, the addition amount of the straw powder in the sodium hydroxide solution is 50-55mg/mL.
5. The method for preparing the gangue modified heavy metal adsorbent as claimed in claim 4, wherein: in S3, the addition amount of the alkalized straw powder in the sodium chlorite solution is 0.08-0.12g/mL.
6. The method for preparing the gangue modified heavy metal adsorbent as claimed in claim 5, wherein: in the step S4, the addition amount of the straw cellulose in the ethanol solution is 0.13-0.15g/mL.
7. The method for preparing the gangue modified heavy metal adsorbent as claimed in claim 6, wherein: in S4, the addition amount of the sodium hydroxide is 6-9% of the mass percentage of the cellulose dispersion liquid.
8. The method for preparing the gangue modified heavy metal adsorbent as claimed in claim 7, wherein: in S4, the addition amount of the chloroacetic acid is 7-8% of the mass percentage of the cellulose dispersion.
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