CN104128161A - Amino-modified active coke heavy metal adsorbent and preparation method thereof - Google Patents
Amino-modified active coke heavy metal adsorbent and preparation method thereof Download PDFInfo
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- CN104128161A CN104128161A CN201310159559.4A CN201310159559A CN104128161A CN 104128161 A CN104128161 A CN 104128161A CN 201310159559 A CN201310159559 A CN 201310159559A CN 104128161 A CN104128161 A CN 104128161A
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Abstract
The invention discloses an amino-modified active coke heavy metal adsorbent and a preparation method thereof. Active coke granules are employed as a base material. Strong-polarity amino groups are introduced onto surfaces of the active coke granules to obtain the adsorbent for adsorbing heavy metal through an esterification reaction between hydroxyl groups on the surfaces of the active coke granules and glycine. The amino-modified active coke heavy metal adsorbent can adsorb various heavy metals such as mercury, nickel, chromium, cadmium, copper, plumbum and the like with a removal ratio reaching 86.1-100.0%.
Description
Technical field
The invention belongs to material for water treatment preparation field, relate to a kind of method that adopts amion acetic acid chemical modification activated coke particle to prepare heavy metal absorbent.
Background technology
Along with the quickening of process of industrialization and the raising of living standards of the people, water pollution problems is on the rise, and receives increasing concern.Heavy metal is a kind of pollutant being extensively present in sewage and drinking water, and serious threat is to biological health.Heavy metal is different with organic pollution, heavy metal can not be biodegradable, just be difficult to be discharged from vitro once enter food chain, even if its concentration in natural environment is very low, through assimilation step by step, storage and the enrichment of food chain biologies at different levels, finally also can in the body of the mankind and other animals, reach quite high concentration, the whole food chain organism especially biology on food chain top is caused to very major injury.For the improvement of heavy metal wastewater thereby, now have multiple improvement technology both at home and abroad, as electricity flocculation, chemical precipitation, ion-exchange, biological adsorption, co-precipitation, absorption, reducing process, coagulation and stable/bearing's logos etc.Process at present that heavy metal in waste water is general adopts traditional physico-chemical process, but when heavy metal concentration is lower, these class methods not only clearance are low, and have that complex process, complex operation, operating cost are high, generation secondary pollution problems.Therefore in the improvement of heavy metal wastewater thereby, problem demanding prompt solution is how can the heavy metal concentration in polluted-water be reduced to harmless level with cost-effective means, thereby eliminates its environmental risk.
Absorption method, because it has the advantages such as raw material source is abundant, cost is low, adsorption plant is simple, easy to operate, secondary pollution is few, is widely used in processing the every field of waste water.Absorption method is mainly concerned with the contact process of solution and adsorbent.Absorbent particles can be removed one or more solutes or store.The main Types of conventional water treatment absorbent can be divided into carbon-bearing adsorbent, inorganic adsorbent, polymer absorbant and other adsorbents.Activated coke is the one of carbon-bearing adsorbent, and it is the porous mass that does not obtain abundant destructive distillation or activation of developing taking brown coal as primary raw material, has absorption and catalysis dual property.Because the existence of resources advantage, activated coke is a kind of advanced treatment of wastewater scavenging material of high performance-price ratio.Compared with active carbon, activated coke not only has advantages of that functional group is abundant, adsorption efficiency is high, and has overcome again that its price is high, mechanical strength is low, the shortcoming of easy pulverizing, has shown more wide application prospect in water treatment.But because the structure of activated coke is taking carbon as main, surface polarity is lower, on the weak side with the binding ability of heavy metal, lower to the adsorption capacity of heavy metal in waste water.In order to improve the adsorption capacity of activated coke to heavy metal, it is a kind of feasible approach that activated coke is carried out to modification processing.The present invention aim to provide a kind of simple chemical modification method by amido modified on activated coke surface, to obtain amino modified active coke adsorbent, this adsorbent is the heavy metal in adsorbed water effectively.Preparation process is carried out at a lower temperature, and without high-temperature heating, the amion acetic acid adopting and acetic anhydride source are abundant, and cost is low, non-secondary pollution.The prepared amino modified active coke adsorbent of the method can effectively be eliminated the harm of heavy metal, and reduces adsorbent cost and processing cost, has higher using value, can play a significant role at field of Environment Protection.
Summary of the invention
The method that the present invention prepares amino modified activated coke heavy metal absorbent has the following step:
(1) a certain amount of acetic anhydride, amion acetic acid and a small amount of concentrated sulfuric acid are mixed in container, wherein the weight ratio of amion acetic acid and acetic anhydride is: 10: 1 ~ 1: 1;
(2) in container described in the first step, add a certain amount of activated coke particle and again mix, wherein the weight ratio of activated coke and acetic anhydride is: 10: 1 ~ 1: 1, the particle diameter of activated coke used was below 40 orders;
(3) container that fills above-mentioned solidliquid mixture is heated to 10 ~ 15 h at 60 ~ 100 DEG C;
(4) solidliquid mixture is taken out and filtered, gained solid matter with deionized water is washed till pH neutral;
(5) the 4th step gained solid product is made to adsorbent after freeze drying 24 ~ 48 h at-70 ~-30 DEG C.
In the described first step, amion acetic acid is solid at normal temperatures, as modifier, in modified-reaction, provide carboxyl, and acetic anhydride and the concentrated sulfuric acid are liquid at normal temperatures, as dehydrating agent and catalyst, three is stirred and is conducive to improve the mass transport process of modified-reaction;
In described second step, activated coke, as skeleton, provides hydroxyl in modified-reaction, is the matrix material of prepared adsorbent;
At 60 ~ 100 DEG C, there is esterification in the carboxyl that the hydroxyl that in described the 3rd step, activated coke provides and amion acetic acid provide, acetic anhydride and the concentrated sulfuric acid play dehydration and catalytic action in this reaction, thereby by amido modified at activated coke particle surface, obtain amino modified activated coke, amino can enhanced activity the polarity on burnt surface, and heavy metal in waste water is combined, be conducive to improve the adsorption efficiency of activated coke particle for heavy metal;
In described the 4th step, filtration and cleaning process are intended to remove the acid impurities such as the surperficial and inner residual amion acetic acid of amino modified activated coke, acetic anhydride, acetic acid, sulfuric acid;
Under be intended to remove amino modified activated coke surface and inner moisture in the 5th step, employing vacuum freeze-drying method, freezes amino modified activated coke at low temperatures, makes moisture wherein by the solid-state gaseous state that is directly sublimed under vacuum state, dehydrates.Whole dry run is carried out under low temperature, low pressure, and moisture directly distils, and amino modified activated coke is not subject to surface tension effects, its institutional framework and surface functional group are preserved preferably, do not have surperficial sclerosis problem, and it inner forms the spongy of porous, be conducive to improve adsorption capacity.
The amino modified activated coke making through this method is graininess, there is higher polarity and larger specific area, to the advantages of good adsorption effect of heavy metal, and the situation that different anions exists can be applicable to, the waste water of the mercury that contains low concentration, nickel, chromium, cadmium, copper and the heavy metal such as plumbous can be processed.
The invention has the advantages that:
1) adsorbent provided by the invention reaches 86.1～100.0 % to mercury, nickel, chromium, cadmium, copper and plumbous adsorption rate, for the processing of heavy metal wastewater thereby especially low concentration heavy metal water provides a kind of novel environment friendly effective water treatment agent;
2) to have particle diameter little and even for adsorbent provided by the invention, and specific area is large, the advantage of advantages of good adsorption effect;
3) under adsorbent normal temperature provided by the invention, have good adsorption capacity, adsorption operations is simple;
4) adsorbent provided by the invention all has good adsorption effect for various heavy, and can in the situation that various heavy coexists, bring into play good effect;
5) adsorbent provided by the invention can be applicable to the more complicated heavy metal wastewater thereby of composition, and adsorption effect is affected not quite by anion;
6) adsorbent provided by the invention utilizes the heavy metal of the difficult low concentration of removing of traditional adsorbent to reach very high removal effect in can be to waste water under lower dosage, and the solid waste of generation is few, can reduce adsorbent cost and subsequent treatment cost;
7) the matrix material activated coke source that the present invention adopts is abundant, and cost is low;
8) the matrix material activated coke mechanical strength that the present invention adopts is high, can tolerate mechanical agitation;
9) the matrix material activated coke that the present invention adopts is difficult for rotting, energy Long-term Storage;
10) the present invention adopts vacuum freeze-drying method, and amino modified activated coke is freezed at low temperatures, makes moisture wherein by the solid-state gaseous state that is directly sublimed under vacuum state, dehydrates.Whole dry run is carried out under low temperature, low pressure, and moisture directly distils, and amino modified activated coke is not subject to surface tension effects, its institutional framework and surface functional group are preserved preferably, do not have surperficial sclerosis problem, and it inner forms the spongy of porous, be conducive to improve adsorption capacity;
11) the present invention adopts chemical mode, and by active coke powder modification, preparation method is simple to operate, does not relate to high temperature and destroys, less on activated coke specific area and internal structure impact;
12) institute of the present invention with medicament amion acetic acid, acetic anhydride wide material sources, cost is lower, and safety non-toxic, can not produce secondary pollution;
13) the chemical modification mode of the activated coke that the present invention adopts is temperature required lower, and energy consumption is less;
14) in the preparation process of adsorbent provided by the invention, equipment needed thereby is simple, and operating process is easily controlled.
Embodiment
embodiment 1:the preparation of amino modified activated coke heavy metal absorbent:
Take 5.0 g amion acetic acids, 1.0 g acetic anhydrides, add 1 concentrated sulfuric acid, in container, mix; Then add 10.0 g activated coke particles (100 orders are following) and again mix; At 60 ~ 70 DEG C, place after 10 h, gained solidliquid mixture is taken out and filtered, it is 5 that gained solid matter with deionized water is washed till pH; By making adsorbent after freeze drying 24 h at gained solid product-70 ~-60 DEG C, in drier, preserve, obtain amino modified activated coke heavy metal absorbent.The amino modified activated coke making through this method is graininess, and recording BET specific area is 156.7 m
2g
-1.
embodiment 2: the absorption to Treating Electroplate Wastewater Containing Nickel:
Take 20.0 g amion acetic acids, 10 g acetic anhydrides, add 3 concentrated sulfuric acids, in container, mix; Then add 20.0 g activated coke particles (80 ~ 100 order) and again mix; At 80 ~ 90 DEG C, place after 15 h, gained solidliquid mixture is taken out and filtered, gained solid matter with deionized water is washed till pH neutrality; By making adsorbent after freeze drying 38 h at gained solid product-60 ~-50 DEG C, in drier, preserve, obtain amino modified activated coke heavy metal absorbent.The amino modified activated coke making through this method is graininess.
Get 100 mL Treating Electroplate Wastewater Containing Nickel, Ni (II) initial concentration is known, be 10.0 mg/L, pH value of solution is 3.8, adds the amino modified activated coke heavy metal absorbent of 0.1 g, velocity fluctuation 15 h with 150 ~ 160 rpm at 30 DEG C in constant-temperature table, then sampling, crosses after 0.45-μ m filter membrane, with Inductively coupled plasma mass spectrometry (ICP-MS, Agilent 7500a, U.S.A.) concentration that records sample solution Ni (II) is 0.8 mg/L.
In order to verify the absorption property of the absorbent particles that the present invention makes, evaluate adsorption effect by clearance, circular is as follows:
Clearance η=(c
0-c
e)/c
0× 100 %
In formula, η is the clearance of adsorbent to Ni (II), and unit is %; c
0for the initial concentration of Ni (II), the mg/L of unit; c
ethe concentration of Ni during for adsorption equilibrium (II), the mg/L of unit.
The clearance that calculates this experiment Ni (II) is 92.0 %, and water outlet Ni (II) concentration is less than 1 mg/L, reaches discharge standard.
embodiment 3: the absorption to cadmium in the situation that cadmium individualism and various heavy coexist:
Take 20.0 g amion acetic acids, 8 g acetic anhydrides, add 3 concentrated sulfuric acids, in container, mix; Then add 20.0 g activated coke particles (60 ~ 100 order) and again mix; At 80 ~ 90 DEG C, place after 13 h, gained solidliquid mixture is taken out and filtered, gained solid matter with deionized water is washed till pH neutrality; By making adsorbent after freeze drying 48 h at gained solid product-60 ~-50 DEG C, in drier, preserve, make amino modified activated coke heavy metal absorbent.
Preparation Cd (NO
3)
2solution, the concentration of Cd (II) is 0.1 mg/L, pH is 8.Preparation Cr (NO
3)
3,ni (NO
3)
2,cu (NO
3)
2,cd (NO
3)
2,pb (NO
3)
2mixed solution, Cr (III), Ni (II), Cu (II), Cd (II), the concentration of Pb (II) is 0.1 mg/L, pH is 8.Get two kinds of each 50 mL of solution, add respectively 5 mg adsorbents, velocity fluctuation 10 h with 150 ~ 170 rpm at 25 DEG C in constant-temperature table, then sampling, cross after 0.45-μ m filter membrane, with Inductively coupled plasma mass spectrometry (ICP-MS, Agilent 7500a, U.S.A.) mensuration Cr (III), Ni (II), Cu (II), Cd (II), the concentration of Pb (II).Calculate this experiment the clearance of Cd (II) in the single solution of cadmium and various heavy mixed solution is respectively to 100.0 ± 0.0 %, 86.1 ± 0.5 %.
Compare with similar adsorbent, the unit volume dosage of this test amino modified activated coke heavy metal absorbent used is only 0.1 g/L, under very little dosage, can in the adsorption process of the cadmium to low concentration, show very high clearance, and in the situation that coexisting, various heavy still can ensure the clearance to cadmium, greatly reduce the cost of required adsorbent, and it is little to produce solid waste, is conducive to subsequent treatment, has very wide application prospect.
embodiment 4: the absorption of the mercury-containing waste water to different initial concentrations
Take 10.0 g amion acetic acids, 8 g acetic anhydrides, add 3 concentrated sulfuric acids, in container, mix; Then add 15.0 g activated coke particles (60 ~ 100 order) and again mix; At 80 ~ 90 DEG C, place after 13 h, gained solidliquid mixture is taken out and filtered, gained solid matter with deionized water is washed till pH neutrality; By making adsorbent after freeze drying 48 h at gained solid product-60 ~-50 DEG C, in drier, preserve, make amino modified activated coke heavy metal absorbent.
For investigating the impact of initial concentration on Hg (II) adsorption process, carry out adsorption isotherm experiment.Prepare the Hg (NO of a series of different initial concentrations
3)
2solution, the concentration of Hg (II) is respectively 10.00,20.00,40.00,60.00,100 mg/L, pH is 5, and adds 10 mM KNO
3for ionic strength.Employing method is similarly to Example 3 to Hg (NO
3)
2solution adsorbs, and measures by the concentration employing Cold Atomic Fluorescent Mercury method of Hg (II), and atomic fluorescence detector model is AF-610B(Beijing Rayleigh Analytical Instrument Co., China).
In order to verify the absorption property of the absorbent particles that the present invention makes, evaluate adsorption effect by equilibrium adsorption capacity, circular is as follows:
Adsorbance q
e=(c
0-c
e) × V/m × 100 %
In formula, q
efor the adsorbance of adsorbent to Hg (II), unit is mg/g; c
0for the initial concentration of Hg (II), the mg/L of unit; c
ethe concentration of Hg during for adsorption equilibrium (II), the mg/L of unit; V is Hg (NO
3)
2the volume of solution, Unit/mL, Hg (NO used in this experiment
3)
2the volume of solution is 50 mL; M is the dosage of adsorbent, the mg of unit, and in this experiment, the dosage of amino modified activated coke heavy metal absorbent used is 5 mg.
Measure through parallel laboratory test, obtain following result:
The adsorbance (mg/g) of the Hg (II) of the amino modified activated coke heavy metal absorbent of table 2 to different initial concentrations
Reach a conclusion by experiment as follows:
Be 10 mM KNO in ionic strength
3situation under, amino modified active coke adsorbent has suction-operated to Hg (II), and adsorbance increases with the rising of Hg (II) initial concentration, and reaches capacity gradually.Measure through parallel laboratory test, in the time that Hg (II) initial concentration is 100.00 mg/L, amino modified active coke adsorbent has reached 542.57 mg/g to the adsorbance of Hg (II), compare with similar adsorbent (42.6 ~ 345.8 mg/g), its saturated extent of adsorption is higher, in Hg (II) waste water treatment process, has significant advantage.
In sum, adopt activated coke particle as matrix material, be graininess by the amino modified activated coke heavy metal absorbent of the prepared graininess of chemical reaction profile, there is particle diameter little and even, the advantage that specific area is large.The method utilizes the hydroxyl on activated coke surface and amion acetic acid to carry out esterification, successfully introduces amino at activated coke particle surface, obtains the adsorbent of Adsorption of Heavy Metals.Modifier amion acetic acid safety non-toxic used, can not cause secondary pollution, and absorbent preparation is simple to operate, with low cost.Amino modified active coke adsorbent of the present invention can be to mercury, nickel, chromium, cadmium, the waste water of copper and the various heavy such as plumbous with and mixed solution process, under normal temperature, there is good adsorption capacity, and can be applicable to the heavy metal wastewater thereby of Various Complex composition, not affected by metal species and interfering ion, adsorption operations is simple, there is good use value and wide should have prospect, for the processing of low-concentration heavy metal in Surface Processing Industry and other industrial wastewaters provides a kind of simple and effective method, this activated coke lower-cost resource is made full use of simultaneously, and open up a kind of method of modifying---chemical modification of effective activated coke, for the industrial applications of adsorbent lays the foundation, realize the new breakthrough of environmental pollution improvement's aspect technology.
Claims (4)
1. one kind is utilized the graininess amino modified activated coke heavy metal absorbent of activated coke as matrix material, it is characterized in that: the main component of described adsorbent is activated coke particle, the amino of successfully introducing at activated coke particle surface in preparation process, the particle diameter of described granular adsorbent is below 40 orders.
2. heavy metal absorbent according to claim 1, is characterized in that: can process the waste water of mercurous, nickel, chromium, cadmium, copper and plumbous heavy metal, its clearance can reach 86.1～100.0 %.
3. prepare a method for adsorbent as claimed in claim 1, it is characterized in that there is following preparation steps:
(1) a certain amount of acetic anhydride, amion acetic acid and a small amount of concentrated sulfuric acid are mixed in container, wherein the weight ratio of amion acetic acid and acetic anhydride is: 10: 1 ~ 1: 1;
(2) in container described in the first step, add a certain amount of activated coke particle and again mix, wherein the weight ratio of activated coke and acetic anhydride is: 10: 1 ~ 1: 1, the particle diameter of activated coke used was below 40 orders;
(3) container that fills above-mentioned solidliquid mixture is heated to 10 ~ 15 h at 60 ~ 100 DEG C;
(4) solidliquid mixture is taken out and filtered, gained solid matter with deionized water is washed till pH neutral;
(5) the 4th step gained solid product is made to adsorbent after freeze drying 24 ~ 48 h at-70 ~-30 DEG C.
4. preparation method according to claim 3, it is characterized in that: in step (1), (2), (3), be to adopt activated coke particle as matrix material, at 60 ~ 100 DEG C, there is esterification with amion acetic acid, and utilize acetic anhydride and the concentrated sulfuric acid as dehydrating agent and catalyst.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104946897A (en) * | 2015-06-08 | 2015-09-30 | 江苏大学 | Method for treating steel plant zinc-containing smoke dust through wet process to realize enrichment of zinc sulfide concentrate |
| CN106914282A (en) * | 2017-03-24 | 2017-07-04 | 马鞍山中创环保科技有限公司 | A kind of fine quick method prepared except nickel ion exchange fiber of utilization cotton |
| CN107686110A (en) * | 2016-08-04 | 2018-02-13 | 中国石油化工股份有限公司 | A kind of activated coke and preparation method thereof |
| CN108203182A (en) * | 2018-01-16 | 2018-06-26 | 南乙环境工程技术（上海）有限公司 | It is a kind of while remove the treatment process and system of total nickel and total cadmium in waste water |
| CN108993504A (en) * | 2018-07-25 | 2018-12-14 | 北京市劳动保护科学研究所 | A kind of modified active coke and preparation method thereof for sulfur-containing smoke gas demercuration |
| CN113318705A (en) * | 2021-07-13 | 2021-08-31 | 榆林学院 | Active coke loaded zero-valent iron nano composite material and preparation method and application thereof |
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| RU2720155C1 (en) * | 2019-07-17 | 2020-04-24 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Петербургский государственный университет путей сообщения Императора Александра I" | Method of purifying waste water from lead ions |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104946897A (en) * | 2015-06-08 | 2015-09-30 | 江苏大学 | Method for treating steel plant zinc-containing smoke dust through wet process to realize enrichment of zinc sulfide concentrate |
| CN107686110A (en) * | 2016-08-04 | 2018-02-13 | 中国石油化工股份有限公司 | A kind of activated coke and preparation method thereof |
| CN106914282A (en) * | 2017-03-24 | 2017-07-04 | 马鞍山中创环保科技有限公司 | A kind of fine quick method prepared except nickel ion exchange fiber of utilization cotton |
| CN106914282B (en) * | 2017-03-24 | 2020-04-03 | 马鞍山中创环保科技有限公司 | Method for rapidly preparing nickel-removing ion exchange fiber by using cotton fiber |
| CN108203182A (en) * | 2018-01-16 | 2018-06-26 | 南乙环境工程技术（上海）有限公司 | It is a kind of while remove the treatment process and system of total nickel and total cadmium in waste water |
| CN108993504A (en) * | 2018-07-25 | 2018-12-14 | 北京市劳动保护科学研究所 | A kind of modified active coke and preparation method thereof for sulfur-containing smoke gas demercuration |
| CN113318705A (en) * | 2021-07-13 | 2021-08-31 | 榆林学院 | Active coke loaded zero-valent iron nano composite material and preparation method and application thereof |
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| CN104128161B (en) | 2018-06-15 |
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Effective date of registration: 20200908 Address after: 215163 building 16, No.158, Jinfeng Road, science and Technology City, Suzhou high tech Zone, Jiangsu Province Patentee after: RESEARCH INSTITUTE FOR ENVIRONMENTAL INNOVATION (SUZHOU) TSINGHUA Address before: 100085 Beijing city Haidian District Shuangqing Road No. 18 Patentee before: Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences |
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