CN113680318A - Preparation method of granular bentonite adsorbent - Google Patents
Preparation method of granular bentonite adsorbent Download PDFInfo
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- CN113680318A CN113680318A CN202110993113.6A CN202110993113A CN113680318A CN 113680318 A CN113680318 A CN 113680318A CN 202110993113 A CN202110993113 A CN 202110993113A CN 113680318 A CN113680318 A CN 113680318A
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- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 title claims abstract description 243
- 239000000440 bentonite Substances 0.000 title claims abstract description 241
- 229910000278 bentonite Inorganic materials 0.000 title claims abstract description 241
- 239000003463 adsorbent Substances 0.000 title claims abstract description 71
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 60
- 238000001179 sorption measurement Methods 0.000 claims abstract description 54
- 239000000843 powder Substances 0.000 claims abstract description 39
- 238000000034 method Methods 0.000 claims abstract description 29
- 239000000853 adhesive Substances 0.000 claims abstract description 24
- 230000001070 adhesive effect Effects 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000003837 high-temperature calcination Methods 0.000 claims abstract description 18
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 11
- 230000004048 modification Effects 0.000 claims abstract description 8
- 238000012986 modification Methods 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 25
- 238000003756 stirring Methods 0.000 claims description 15
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 14
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 14
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 14
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 14
- 238000007873 sieving Methods 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 11
- 150000003242 quaternary ammonium salts Chemical group 0.000 claims description 10
- 239000003607 modifier Substances 0.000 claims description 7
- 239000012266 salt solution Substances 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 5
- 239000002957 persistent organic pollutant Substances 0.000 claims description 5
- 238000012216 screening Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 4
- 229920001661 Chitosan Polymers 0.000 claims description 2
- 229920000858 Cyclodextrin Polymers 0.000 claims description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- 229920002472 Starch Polymers 0.000 claims description 2
- 239000011230 binding agent Substances 0.000 claims description 2
- 239000008240 homogeneous mixture Substances 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 235000019422 polyvinyl alcohol Nutrition 0.000 claims description 2
- HFHDHCJBZVLPGP-UHFFFAOYSA-N schardinger α-dextrin Chemical compound O1C(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(O)C2O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC2C(O)C(O)C1OC2CO HFHDHCJBZVLPGP-UHFFFAOYSA-N 0.000 claims description 2
- 239000008107 starch Substances 0.000 claims description 2
- 235000019698 starch Nutrition 0.000 claims description 2
- 238000001354 calcination Methods 0.000 abstract description 11
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 abstract description 10
- 230000008569 process Effects 0.000 abstract description 10
- 239000002994 raw material Substances 0.000 abstract description 9
- 230000007613 environmental effect Effects 0.000 abstract description 6
- 229910002092 carbon dioxide Inorganic materials 0.000 abstract description 5
- 239000001569 carbon dioxide Substances 0.000 abstract description 5
- 238000010923 batch production Methods 0.000 abstract description 4
- 239000012535 impurity Substances 0.000 abstract description 4
- 239000011800 void material Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 30
- 239000004098 Tetracycline Substances 0.000 description 15
- 229960002180 tetracycline Drugs 0.000 description 15
- 229930101283 tetracycline Natural products 0.000 description 15
- 235000019364 tetracycline Nutrition 0.000 description 15
- 150000003522 tetracyclines Chemical class 0.000 description 15
- 230000000694 effects Effects 0.000 description 9
- 230000006872 improvement Effects 0.000 description 9
- 239000011229 interlayer Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 229960000907 methylthioninium chloride Drugs 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 230000036571 hydration Effects 0.000 description 4
- 238000006703 hydration reaction Methods 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 150000001768 cations Chemical class 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- 239000002352 surface water Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Chemical group [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 229910052901 montmorillonite Inorganic materials 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
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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
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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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/12—Naturally occurring clays or bleaching earth
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28016—Particle form
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- 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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3042—Use of binding agents; addition of materials ameliorating the mechanical properties of the produced sorbent
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- 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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing
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- 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
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- 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
- C02F2101/30—Organic compounds
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- Water Supply & Treatment (AREA)
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Abstract
The invention provides a preparation method of a granular bentonite adsorbent, which comprises the steps of adding carbon-containing powder into bentonite as a raw material, adding the raw material into an adhesive solution to prepare viscous bentonite, drying, and then calcining at high temperature under an aerobic condition to prepare the granular bentonite adsorbent; and carrying out surface modification treatment to obtain the modified granular bentonite adsorbent. Wherein, the added carbon-containing powder is decomposed into carbon dioxide during high-temperature calcination, so that the bentonite has more adsorption sites, and the adsorption capacity of the granular bentonite is improved; the addition of the adhesive ensures that the bentonite is not easy to collapse during calcination, and the strength of the granular bentonite is improved; the high-temperature calcination process can remove water and impurities in the bentonite, increase the specific surface area of the bentonite, loosen the void structure of the bentonite and improve the adsorbability of the bentonite. The preparation process is simple and easy for batch production; the prepared granular bentonite adsorbent has the characteristics of good adsorption performance, high strength, good environmental protection, no secondary pollution, wide application range and the like.
Description
Technical Field
The invention relates to the technical field of bentonite adsorption, in particular to a preparation method of a granular bentonite adsorbent.
Background
The bentonite is a non-metallic mineral resource with montmorillonite as a main mineral component, and due to a special two-dimensional space structure formed by montmorillonite unit cells, the bentonite has the condition that the action of certain cations and montmorillonite unit cells is unstable and is easy to exchange with other cations, so that the bentonite has better ion exchange property and adsorption property. We refer to the phenomenon of aggregation of certain molecules on the surface of bentonite as adsorption of bentonite. The bentonite as the adsorbing material has the advantages of low price, rich reserves, environmental protection, large adsorption capacity and the like, and the adsorption effect is widely applied in industry. For example, the drilling mud often utilizes the adsorption characteristic of bentonite minerals to adjust mud parameters of different use purposes, for example, a filtrate reducer is added, one end of a high molecular polymer is adsorbed on the surface of bentonite particles, and the other end of the high molecular polymer is dissolved in water, so that the bentonite particles and water molecules generate an indirect connection to form a bridging effect, free water in the mud is reduced, the performance parameters of the mud are changed, and the purpose of reducing the filtrate loss is achieved.
The bentonite is applied to manufacturing the adsorbing material due to good adsorption performance, and when the bentonite is used for adsorption in a water environment, the bentonite has strong hygroscopicity and expansibility, so that water with volume being 8-15 times of that of the bentonite can be adsorbed, and the volume expansion can reach several times to 30 times; can be dispersed into a gelatinous state and a suspended state in an aqueous medium, and the medium solution has certain viscosity; therefore, the powdered bentonite is difficult to separate from water after adsorbing and removing pollutants, so that secondary pollution is caused, and the application of the bentonite is limited. The prior scholars try to prepare granular bentonite and improve the separability of the granular bentonite. However, when bentonite particles are directly prepared from bentonite powder, the bentonite particles are not high in strength because the bentonite itself is not strong in cohesiveness, so that the bentonite particles are easy to collapse in the calcining process.
In addition, the surface silica and alumina structures of the bentonite have extremely strong hydrophilicity, and the bentonite cannot effectively adsorb organic matters due to the existence of interlayer exchangeable cation hydration; permanent negative charges existing between bentonite layers also make the bentonite layers incapable of adsorbing anionic pollutants; the bentonite has the function of adsorbing heavy metal ions, but is easy to desorb and difficult to completely remove from the water body. Therefore, the bentonite is modified to change the surface property and the interlayer structure, so that the adsorption capacity, the adsorption selectivity and the adsorption stability are improved, and the bentonite can be better used for actual production.
In view of the above, there is a need to design an improved method for preparing a granular bentonite adsorbent to solve the above problems.
Disclosure of Invention
The invention aims to provide a preparation method of a granular bentonite adsorbent, and the granular bentonite adsorbent prepared by the method has the characteristics of good adsorption performance, good environmental protection, simple process preparation, wide application range and the like; the problems that the existing bentonite adsorption material is difficult to separate from water, is easy to cause secondary pollution, can not effectively adsorb hydrophobic organic pollutants, and is limited in application due to low strength during calcination of the granular bentonite are solved.
In order to achieve the above object, the present invention provides a method for preparing a granular bentonite adsorbent, comprising the following steps:
s1, sieving the bentonite powder and the carbon-containing powder respectively, and then fully mixing the bentonite powder and the carbon-containing powder to obtain a uniform mixture of the bentonite powder and the carbon-containing powder;
s2, adding the bentonite and carbon-containing powder mixed material prepared in the step S1 into an adhesive solution under the condition of stirring, and stirring for 5-10 min to obtain viscous bentonite;
s3, drying the viscous bentonite prepared in the step S2 for 4-6 hours, then carrying out high-temperature calcination under an aerobic condition, and finally crushing and screening to obtain the granular bentonite adsorbent.
As a further improvement of the present invention, the preparation method further comprises: and (4) adding the granular bentonite adsorbent obtained in the step (S3) into a modifier for surface modification, washing with water, and drying to obtain the modified granular bentonite adsorbent.
In a further improvement of the present invention, in step S1, the mass fraction of the carbonaceous powder in the homogeneous mixture is 10 to 30%, and the carbonaceous powder is activated carbon powder.
In a further improvement of the present invention, in step S2, the mass fraction of the solute in the adhesive solution is 5 to 10%.
As a further improvement of the invention, in step S3, the temperature of the high-temperature calcination is 500-700 ℃ and the time is 1-2 h.
As a further improvement of the invention, the solute of the adhesive solution is one or more of carboxymethyl cellulose, polyvinyl alcohol, carboxymethyl cellulose, soluble starch, chitosan and cyclodextrin.
As a further improvement of the invention, the mass ratio of the solute in the modifier solution to the granular bentonite is (0.5-1): 1.
As a further improvement of the invention, the modifier is a quaternary ammonium salt solution to enhance the adsorption performance of the granular bentonite on organic pollutants.
In a further improvement of the present invention, in step S1, the screening is performed by sieving the bentonite powder and the carbonaceous powder with 100 to 120 mesh sieves, respectively.
In a further improvement of the present invention, in step S3, the screening is performed by sieving the crushed bentonite lumps through a 20-40 mesh sieve.
The invention has the beneficial effects that:
1. the invention provides a preparation method of a granular bentonite adsorbent, which is characterized in that bentonite powder and carbon-containing powder are mixed according to a certain proportion and used as raw materials of the adsorbent, the raw materials are added into an adhesive solution to prepare viscous bentonite, and then the viscous bentonite is calcined at high temperature to prepare the granular bentonite adsorbent. The method has simple process and is easy for batch production; the carbon-containing powder added in the preparation process is decomposed into carbon dioxide to be removed under the aerobic condition during subsequent high-temperature calcination, so that the internal gaps of the granular bentonite are richer, the specific surface area of the granular bentonite is improved, the prepared granular bentonite has more adsorption sites, and the adsorption capacity of the granular bentonite is improved; the prepared granular bentonite adsorbent has better adsorption effect and better adsorption performance.
2. When the granular bentonite adsorbent is prepared, the mixed raw material of bentonite powder and carbon-containing powder is added into the solution of the adhesive; by adding the adhesive, on one hand, the cohesiveness of the granular bentonite is improved, and the granular bentonite is not easy to collapse during subsequent high-temperature calcination, so that the prepared granular bentonite has higher strength; on the other hand, the carboxymethyl cellulose is decomposed during high-temperature calcination, the problem of blocking an adsorption pore channel of the granular bentonite is avoided, the adsorption capacity and effect of an adsorbent prepared from the granular bentonite are not influenced, and the gas generated by decomposition can improve the internal porosity of the granular bentonite to a certain extent, so that the adsorption performance of the granular bentonite is improved.
3. According to the invention, the surface modification treatment is carried out on the granular bentonite adsorbent, the modifier is embedded into the interlayer of the bentonite, and the hydrophilicity of the surface of the bentonite is converted into hydrophobicity, so that the content of organic carbon in the bentonite is increased, the interlayer spacing of the bentonite is increased, the affinity and adsorption capacity of the bentonite to organic matters are favorably improved, and the removal rate of the bentonite to organic pollutants is favorably improved; meanwhile, the surface of the bentonite is changed into hydrophobicity, so that the bentonite is easy to separate from water after adsorption is finished, secondary pollution is avoided, and the adsorbent prepared from the granular bentonite has environmental protection.
4. The high-temperature calcination process can remove surface water, hydration water and structural bound water of the bentonite and impurities in gaps, increase the specific surface area of the bentonite, loosen the gap structure of the bentonite and improve the adsorption performance of the bentonite.
Drawings
Fig. 1 is a specific flow chart of a preparation method of the granular bentonite adsorbent.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in detail with reference to the accompanying drawings and specific embodiments.
It should be noted that, in order to avoid obscuring the present invention with unnecessary details, only the structures and/or processing steps closely related to the aspects of the present invention are shown in the drawings, and other details not closely related to the present invention are omitted.
In addition, it is also to be noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Referring to fig. 1, a method for preparing a granular bentonite adsorbent includes the following steps:
s1, sieving the bentonite powder and the activated carbon powder by a sieve of 100-200 meshes respectively, and then fully mixing the bentonite powder and the activated carbon powder according to the proportion of 70-90% and the activated carbon of 10-30% to obtain a uniformly mixed material of the bentonite and the activated carbon;
s2, adding the bentonite and activated carbon mixed material prepared in the step S1 into a carboxymethyl cellulose adhesive solution with the concentration of 50-100 g/L under the condition of stirring, and stirring for 5-10 min to obtain viscous bentonite;
preferably, carboxymethyl cellulose is used as an adhesive, so that on one hand, the cohesiveness of the granular bentonite is improved, and the granular bentonite is not easy to collapse during subsequent high-temperature calcination, so that the prepared granular bentonite has higher strength; on the other hand, the carboxymethyl cellulose is decomposed during high-temperature calcination, the problem of blocking an adsorption pore channel of the granular bentonite is avoided, the adsorption capacity and effect of an adsorbent prepared from the granular bentonite are not influenced, and the gas generated by decomposition can improve the internal porosity of the granular bentonite to a certain extent, so that the adsorption performance of the granular bentonite is improved.
S3, drying the viscous bentonite prepared in the step S2 at 100 ℃ for 4-6 hours, then calcining at 500-700 ℃ for 1-2 hours at high temperature under aerobic condition, crushing, sieving with a 20-40 mesh sieve, and screening to obtain granular bentonite;
the high-temperature calcination process can remove surface water, hydration water and structural bound water of the bentonite and impurities in gaps, increase the specific surface area of the bentonite, loosen the gap structure of the bentonite and improve the adsorption performance; meanwhile, the carboxymethyl cellulose is gradually decomposed at high temperature, so that the adsorption pore channel of the granular bentonite cannot be blocked due to adhesion; the carbon powder wrapped in the carboxymethyl cellulose is also subjected to aerobic combustion to generate gases such as carbon dioxide and the like, and the gases escape from the pores of the bentonite, so that the specific surface area of the bentonite is increased.
S4, adding the granular bentonite prepared in the step S3 into a quaternary ammonium salt solution with the concentration of 100-200 mg/L for surface modification, stirring for 1-2 h, filtering, washing for 2-3 times by using deionized water, and drying at 100 ℃ to obtain the granular bentonite adsorbent.
Wherein the mass ratio of the quaternary ammonium salt to the granular bentonite in the quaternary ammonium salt solution is (0.5-1): 1, and in a specific embodiment, 20g of the prepared granular bentonite is added into 100mL of the quaternary ammonium salt solution with the concentration of 100-200 mg/L.
Specifically, bentonite powder and activated carbon powder are mixed according to a certain proportion to serve as raw materials of the adsorbent, the raw materials are added into an adhesive solution to prepare viscous bentonite, and then high-temperature calcination and surface modification are carried out to prepare the adsorbent of granular bentonite. The method has simple process and is easy for batch production; and the activated carbon powder added in the preparation process is decomposed into carbon dioxide to be removed under the aerobic condition during subsequent high-temperature calcination, so that the internal gaps of the granular bentonite are richer, the specific surface area of the granular bentonite is improved, the prepared granular bentonite has more adsorption sites, the adsorption capacity of the granular bentonite is improved, and the adsorption effect and the adsorption performance of the granular bentonite adsorbent are better.
Particularly, the granular bentonite is subjected to surface modification treatment by using quaternary ammonium salt, the quaternary ammonium salt is embedded into a bentonite interlayer, and the hydrophilicity of the surface of the bentonite is converted into hydrophobicity, so that the content of organic carbon in the bentonite is increased, the interlayer spacing of the bentonite is increased, the affinity and adsorption capacity of the bentonite to organic matters are favorably improved, and the removal rate of the bentonite to organic pollutants is favorably improved; meanwhile, the surface of the bentonite is changed into hydrophobicity, so that the bentonite is easy to separate from water after adsorption is finished, secondary pollution is avoided, and the adsorbent prepared from the granular bentonite has environmental protection.
Example 1
The preparation method of the granular bentonite adsorbent provided by the embodiment comprises the following steps:
s1, firstly, sieving bentonite powder and activated carbon powder by a 120-mesh sieve, and then fully mixing 30% of activated carbon and 70% of bentonite powder by mass fraction to obtain a uniformly mixed material;
s2, adding 5g of carboxymethyl cellulose into 100mL of deionized water, uniformly stirring to obtain a uniform mixed solution, adding the uniform mixed material obtained in the step S1 into the carboxymethyl cellulose solution under the stirring condition, and stirring for 10min to obtain viscous bentonite;
s3, drying the viscous bentonite obtained in the step S2 at 100 ℃ for 4 hours to obtain blocky bentonite, calcining the blocky bentonite at 600 ℃ under aerobic condition for 2 hours, taking out and crushing the blocky bentonite, and sieving the blocky bentonite with a 20-mesh sieve to obtain a granular bentonite adsorbent;
s4, preparing 100mL of quaternary ammonium salt solution with the concentration of 200mg/L, adding 20g of prepared granular bentonite, stirring for 2h, filtering, washing the surface of the granular bentonite 3 times by deionized water, and drying for 2h at the temperature of 100 ℃ to prepare the modified bentonite granular adsorbent.
And (4) carrying out strength detection on the granular bentonite adsorbent prepared in the step S3.
100mL of a tetracycline solution with the concentration of 2mg/L is prepared, 5g of the granular bentonite prepared in the step S4 is added thereto, and the mixture is stirred for 2 hours to test the removal rate of tetracycline in the tetracycline solution.
Comparative example 1
Compared with example 1, the difference of the preparation method of the granular bentonite adsorbent provided in comparative example 1 is that no activated carbon is added in comparative example 1, and the rest is the same as that in example 1, and detailed description is omitted here.
Comparative example 2
Compared with example 1, the difference of the preparation method of the granular bentonite adsorbent provided in comparative example 2 is that no adhesive is added in comparative example 1, and the rest is the same as that in example 1, and detailed description is omitted here.
Compared with the preparation method of the granular bentonite adsorbent in the example 1, the preparation method of the granular bentonite adsorbent in the comparative example 3 is different in that no activated carbon or adhesive is added in the comparative example 1; the rest is the same as that of embodiment 1, and is not described herein.
The strength results of granular bentonite measured in example 1 and comparative examples 1 to 3, which are dimensionless processed with the strength value of comparative example 3 as 100%, and the removal rate of tetracycline from the tetracycline solution were analyzed, and the strength data of all the following examples and comparative examples were processed in this way. The test results of example 1 and comparative examples 1 to 3 are shown in the following table.
TABLE 1 test results of example 1 and comparative examples 1 to 3
| Examples | Activated carbon mass fraction (%) | Adhesive concentration (g/L) | Strength (%) | Tetracycline removal rate (%) |
| Example 1 | 30 | 50 | 160 | ＞95 |
| Comparative example 1 | 0 | 50 | 300 | 73 |
| Comparative example 2 | 30 | 0 | 80 | 87 |
| Comparative example 3 | 0 | 0 | 100 | 52 |
As can be seen from Table 1, the removal rate of tetracycline by the adsorbent prepared from the granular bentonite to which 30% of activated carbon was added in example 1 was 95% or more, while the removal rate of tetracycline by the adsorbent prepared from the granular bentonite to which no activated carbon was added in comparative examples 1 and 3 was significantly lower than that of example 1. The method has the advantages that when the granular bentonite adsorbent is prepared, the active carbon is added, so that the internal gaps of the granular bentonite are richer, the specific surface area of the granular bentonite is improved, the prepared granular bentonite has more adsorption point positions, the adsorption capacity of the granular bentonite is improved, and the adsorption effect and the adsorption performance of the granular bentonite adsorbent are better. While the tetracycline removal results of comparative examples 1 and 3 demonstrate that the addition of the binder to the granular bentonite has a beneficial effect on its adsorption performance. The gas generated by decomposition of the adhesive during high-temperature calcination can also improve the internal porosity of the granular bentonite to a certain extent, so that the adsorption performance of the granular bentonite is improved.
As can be seen from the strength results in Table 1, the strength of the granular bentonite is affected by adding the activated carbon alone in the comparative example 2, but the strength of the granular bentonite is obviously improved after adding the adhesive; comparative example 1 the strength of granular bentonite when only adhesive was added was 3 times the strength of comparative example 3. The results show that when the granular bentonite adsorbent is prepared, the addition of the adhesive can ensure that the granular bentonite adsorbent is not easy to collapse during calcination, the bonding force among bentonite molecules is increased, and the strength of the granular bentonite adsorbent is improved.
Examples 2 to 5
The difference between the preparation methods of particulate bentonite adsorbents provided in examples 2 to 5 and example 1 is that the mass fractions of the added activated carbon powders are different, the mass fractions of the added activated carbon powders in examples 2 to 5 are 10%, 15%, 20% and 25%, respectively, and the rest are the same as those in example 1, and thus, the details are not repeated herein.
The strength of granular bentonite obtained in examples 2 to 5 and the removal rate of tetracycline from the tetracycline solution were analyzed, and the results are shown in the following table.
Table 2 test results for examples 2-5
| Examples | Activated carbonMass fraction (%) | Strength (%) | Tetracycline removal rate (%) |
| Example 2 | 10 | 270 | 81 |
| Example 3 | 15 | 230 | 83 |
| Example 4 | 20 | 200 | 87 |
| Example 5 | 25 | 180 | 92 |
As can be seen from table 2, when the adhesive concentration of examples 2 to 5 was constant, the increase in the mass fraction of activated carbon gradually increased the tetracycline removal rate of the prepared granular bentonite adsorbent, indicating that the adsorption performance of granular bentonite was improved.
Example 6
The preparation method of the granular bentonite adsorbent provided by the embodiment comprises the following steps:
s1, firstly, sieving bentonite powder and activated carbon powder by a 100-mesh sieve, and then fully mixing 30% of activated carbon and 70% of bentonite powder by mass fraction to obtain a uniformly mixed material;
s2, adding 8g of carboxymethyl cellulose into 100mL of deionized water, uniformly stirring to obtain a uniform mixed solution, adding the uniform mixed material obtained in the step S1 into the carboxymethyl cellulose solution under the stirring condition, and stirring for 10min to obtain viscous bentonite;
s3, drying the viscous bentonite obtained in the step S2 at 100 ℃ for 6 hours to obtain blocky bentonite, calcining the blocky bentonite at 500 ℃ under aerobic condition for 1.5 hours, taking out the blocky bentonite, crushing the blocky bentonite, and sieving the blocky bentonite with a 40-mesh sieve to obtain a granular bentonite adsorbent;
s4, preparing 100mL of quaternary ammonium salt solution with the concentration of 100mg/L, adding 20g of prepared granular bentonite, stirring for 1h, filtering, washing the surface of the granular bentonite for 3 times by deionized water, and drying for 2h at the temperature of 100 ℃ to prepare the modified bentonite granular adsorbent.
And (4) carrying out strength detection on the granular bentonite adsorbent prepared in the step S3.
100mL of methylene blue solution with the concentration of 5mg/L is prepared, 5g of the granular bentonite prepared in the step S4 is added into the solution, the mixture is stirred for 1 hour, and the removal rate of methylene blue in the methylene blue solution is tested.
Comparative example 4
The difference between the preparation method of the granular bentonite adsorbent provided in the comparative example 4 and the preparation method of the granular bentonite adsorbent provided in the example 6 is that no activated carbon is added in the comparative example 4, and the rest is the same as that in the example 6, and the details are not repeated herein.
Comparative example 5
The difference between the preparation method of the granular bentonite adsorbent provided in the comparative example 5 and the preparation method of the granular bentonite adsorbent provided in the example 6 is that no adhesive is added in the comparative example 5, and the rest is the same as that in the example 6, and the description is omitted.
The strength of granular bentonite measured in example 6 and comparative examples 4 to 5 and the removal rate of tetracycline from tetracycline solution were analyzed, and the test results are shown in the following table.
Table 3 test results of example 6 and comparative examples 4 to 5
As can be seen from table 3, the removal rate of methylene blue of the adsorbent prepared from 30% activated carbon-added granular bentonite in example 6 was 98% or more, while the removal rate of methylene blue of the adsorbent prepared from activated carbon-free granular bentonite in comparative example 4 was significantly lower than that of example 6. The explanation shows that when the granular bentonite adsorbent is prepared, the adsorption effect and the adsorption performance of the granular bentonite adsorbent are better by adding the activated carbon.
In summary, the invention provides a preparation method of a granular bentonite adsorbent, which comprises the steps of adding activated carbon into bentonite as a raw material, adding the raw material into an adhesive solution to prepare viscous bentonite, and then calcining at a high temperature to obtain the granular bentonite adsorbent; the modified granular bentonite adsorbent is prepared by surface modification. The activated carbon powder added in the preparation process is decomposed into carbon dioxide to be removed under the aerobic condition during subsequent high-temperature calcination, so that the internal gaps of the granular bentonite are richer, the specific surface area of the granular bentonite is improved, the prepared granular bentonite has more adsorption sites, the adsorption capacity of the granular bentonite is improved, and the adsorption effect and the adsorption performance of the granular bentonite adsorbent are better; the addition of the adhesive ensures that the bentonite is not easy to collapse during calcination, and the strength of the granular bentonite is improved; the high-temperature calcination process can remove surface water, hydration water and structural bound water of the bentonite and impurities in gaps, increase the specific surface area of the bentonite, loosen the gap structure of the bentonite and improve the adsorption performance. The preparation process is simple and easy for batch production; the prepared granular bentonite adsorbent has the characteristics of good adsorption performance, high strength during calcination, good environmental protection, no secondary pollution, wide application range and the like.
Although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof without departing from the spirit and scope of the present invention.
Claims (10)
1. The preparation method of the granular bentonite adsorbent is characterized by comprising the following steps:
s1, sieving the bentonite powder and the carbon-containing powder respectively, and then fully mixing the bentonite powder and the carbon-containing powder to obtain a uniform mixture of the bentonite powder and the carbon-containing powder;
s2, adding the bentonite and carbon-containing powder mixed material prepared in the step S1 into an adhesive solution under the condition of stirring, and stirring for 5-10 min to obtain viscous bentonite;
s3, drying the viscous bentonite prepared in the step S2 for 4-6 hours, then carrying out high-temperature calcination under an aerobic condition, and finally crushing and screening to obtain the granular bentonite adsorbent.
2. The method of claim 1, wherein the method further comprises: and (4) adding the granular bentonite adsorbent obtained in the step (S3) into a modifier for surface modification, washing with water, and drying to obtain the modified granular bentonite adsorbent.
3. The method of claim 1, wherein in step S1, the mass fraction of the carbonaceous powder in the homogeneous mixture is 10-30%, and the carbonaceous powder is activated carbon powder.
4. The method for preparing the granular bentonite adsorbent according to claim 1, wherein in the step S2, the mass fraction of the solute in the adhesive solution is 5-10%.
5. The method of claim 1, wherein in step S3, the high temperature calcination is performed at 500-700 ℃ for 1-2 h.
6. The method of claim 4, wherein the solute of the binder solution is one or more of carboxymethyl cellulose, polyvinyl alcohol, carboxymethyl cellulose, soluble starch, chitosan, and cyclodextrin.
7. The method for preparing the granular bentonite adsorbent according to claim 2, wherein the mass ratio of the solute in the modifier solution to the granular bentonite is (0.5-1): 1.
8. The method for preparing the granular bentonite adsorbent according to claim 2, wherein the modifier is a quaternary ammonium salt solution to enhance the adsorption performance of the granular bentonite on the organic pollutants.
9. The method of claim 1, wherein in step S1, the sieving is performed by sieving the bentonite powder and the carbonaceous powder with 100-120 mesh sieves respectively.
10. The method of claim 1, wherein in step S3, the step of sieving is performed by sieving the crushed bentonite lumps through a 20-40 mesh sieve.
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