CN109499543A - A kind of preparation method for the modified activated carbon handling Pb In Exhausted Water ion - Google Patents

A kind of preparation method for the modified activated carbon handling Pb In Exhausted Water ion Download PDF

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Publication number
CN109499543A
CN109499543A CN201811289212.0A CN201811289212A CN109499543A CN 109499543 A CN109499543 A CN 109499543A CN 201811289212 A CN201811289212 A CN 201811289212A CN 109499543 A CN109499543 A CN 109499543A
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China
Prior art keywords
active carbon
handling
modified activated
carbon
activated carbon
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CN201811289212.0A
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Inventor
宋小利
任鑫
高立国
王丹
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Yulin University
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Yulin University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20Solid 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/288Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/20Heavy metals or heavy metal compounds

Abstract

The invention discloses a kind of preparation method of modified activated carbon for handling Pb In Exhausted Water ion, this method is made by impregnating apricot shell active carbon in citric acid solution, after drying by the apricot shell active carbon of citric acid-modified;Preparation method of the invention is simple, and cost is relatively low, and the apricot shell active carbon prepared removes the effect of leaded solion than by the prior art strong by the active carbon of acid or alkali modification removing ability.In addition in existing method of modifying, chemical precipitation method condition is stringent, it is necessary to which strict control pH value, condition is more loose by comparison by the present invention, easily reaches, easily implements;Ion-exchange higher cost, the present invention greatly reduce cost;Gas floatation process takes up a large area, and is only applicable to the lower lead waste water of concentration for the treatment of, and not only occupied area is small by the present invention, but also is suitable for the processing of the lead waste water of various concentration;And the present invention is more efficient than common acid, alkali modification active carbon.

Description

A kind of preparation method for the modified activated carbon handling Pb In Exhausted Water ion
[technical field]
The invention belongs to handle lead waste water field, a kind of modified activated carbon of processing Pb In Exhausted Water ion is related generally to Preparation method.
[background technique]
Lead and lead-containing compounds are one of the toxic chemical substances in pollutant list, in industry plating, paint, plastics combustion All contain a large amount of lead in the flue gas of burning, vehicle exhaust, very harmful to environment and life entity, lead ion is easy in animals and plants Accumulation in vivo has very high toxicity, has more serious influence to human health and animal and plant growth, be considered as a kind of cause Cancer substance.The major toxicity of lead is to will lead to anaemia, lead to reproductive system damage and injury of kidney.Therefore how significantly more efficient The lead ion in waste water is removed, reduces environmental pollution, protecting our living environments is a urgent problem to be solved.
The method of processing lead waste water has at present: chemical precipitation method, ion-exchange and electroosmose process etc..Chemical precipitation method Current most widely used lead containing wastewater treatment technology, by adding lye or sulfide, generate indissoluble lead hydroxide or Vulcanized lead precipitating.But lead is amphoteric metal, it is more stringent using chemical precipitation method control condition.Ion-exchange processing is leaded Waste water, removal rate are high, and effluent quality is good, but be only capable of processing ionic state lead or lead compound and processing cost it is higher.
Active carbon (AC) has unique pore structure and surface chemistry, is a kind of high-efficiency adsorbent, to all kinds of inorganic, organic Object all has preferable adsorption effect, but since active carbon is non-renewable resources, and less varieties, with low content of technology, so Constrain the further development and application of China's activated carbon industry.In order to improve its adsorption capacity, using acidification, basification etc. Method has carried out surface chemical modification to active carbon, can expand the scope of application of active carbon, reduce use cost, improves utilization Rate.But specific research is had no for the active carbon of removal lead ion.
[summary of the invention]
It is an object of the invention to overcome the above-mentioned prior art, a kind of modification for handling Pb In Exhausted Water ion is provided The preparation method of active carbon.This method is modified active carbon by citric acid, and it is useless to improve the activated carbon adsorption being modified The concentration of lead ion in water.
In order to achieve the above objectives, the present invention is achieved by the following scheme:
A kind of preparation method for the modified activated carbon handling Pb In Exhausted Water ion, includes the following steps, will be pretreated The active carbon of 5.0g is immersed in the citric acid solution that mass concentration is 10%, is taken out after immersion, is rushed repeatedly by deionized water Active carbon is washed to the pH value of flushing liquor to filter after neutrality, obtained active carbon drying will be filtered, be made after dry by citric acid Modified active carbon, for the modified activated carbon for handling Pb In Exhausted Water ion.
A further improvement of the present invention is that:
Preferably, the preparation method of pretreated active carbon is the following steps are included: wash commercially available work by deionized water Property charcoal several times, until there is lamination in active carbon and deionized water;Active carbon is taken out, after active carbon for the first time drying, powder It is broken, be ground up, sieved, after the active carbon of sieving is cleaned with deionized water, it is dry to take out active carbon second, is made pretreated Active carbon.
Preferably, active carbon is dry for the first time and second of dry drying temperature is 70 DEG C, and drying time is 12h。
Preferably, the sieving standard of active carbon is 60 mesh.
Preferably, active carbon selects apricot shell active carbon.
Preferably, the preparation process of 10% citric acid solution is to mix 2.1042g lemon granulates with deionized water, Prepare the citric acid solution that mass concentration is 10%.
Preferably, soaking time of the active carbon in 10% citric acid solution is 4h.
Preferably, the drying temperature of filtered active carbon is 70 DEG C, drying time 12h.
Compared with prior art, the invention has the following advantages:
The invention discloses a kind of preparation methods of modified activated carbon for handling Pb In Exhausted Water ion, and this method is by by apricot After shell active carbon impregnates in citric acid solution, is dry, it is made by the apricot shell active carbon of citric acid-modified;Preparation side of the invention Method is simple, and cost is relatively low, and the apricot shell active carbon prepared removes the effect ratio of leaded solion by the prior art sour Or the active carbon removing ability of alkali modification is strong.In addition in existing method of modifying, chemical precipitation method condition is stringent, it is necessary to stringent control PH value processed, condition is more loose by comparison by the present invention, easily reaches, easily implements;Ion-exchange higher cost, the present invention is significantly It reduces costs;Gas floatation process takes up a large area, and is only applicable to the lower lead waste water of concentration for the treatment of, the present invention not only occupied area It is small, and it is suitable for the processing of the lead waste water of various concentration;And active carbon produced by the present invention is more living than common acid, alkali modification Property charcoal is more efficient.
[Detailed description of the invention]
Fig. 1 is that the SEM of unmodified apricot shell active carbon of the invention schemes;
Fig. 2 is that the SEM of the apricot shell active carbon of the invention by citric acid-modified schemes;
Fig. 3 is of the invention by HNO3The SEM of modified apricot shell active carbon schemes;
Fig. 4 is that the SEM of the apricot shell active carbon of the invention being modified by NaOH schemes;
Fig. 5 is that the SEM of the apricot shell active carbon of the invention being modified by KOH schemes;
Fig. 6 is the standard curve determined by atomic absorption spectrophotometry degree flame method.
[specific embodiment]
The invention will be described in further detail with reference to the accompanying drawing:
Embodiment 1
(1) Pre-Treatment of Activated charcoal: washing commercially available active carbon for several times by deionized water, until active carbon and deionized water have point Layer phenomenon stops cleaning, removes the deionized water of layering, and by active carbon, dry 12h taking-up is ground into 70 DEG C of thermostatic drying chambers Powder is screened through 60 mesh sieve, is cleaned being rinsed less than the active carbon of 60 mesh with a large amount of water.Finally, the active carbon handled well is existed Dry 12h is toasted in 70 DEG C of thermostatic drying chambers, is placed on spare in dry flask, and it is apricot shell active carbon that active carbon, which is selected, is denoted as GAC.Fig. 1 is that the SEM of unmodified apricot shell active carbon schemes, it can be seen from the figure that there are many ellipses for unmodified active carbon Aperture, surface smoother.
(2) modifying agent is prepared
It weighs 2.1042g lemon granulates to mix with deionized water, prepares the C that mass concentration is 10%6H8O7·H2O is molten Liquid is denoted as 10%C6H8O7·H2O;
(3) modified activated carbon:
Active carbon in step (1) by pretreated 5.0g is immersed in 10% C prepared in step (2)6H8O7· H2It in O solution, takes out after impregnating 4h, by the pH value of deionized water repeated flushing to flushing liquor to be filtered after neutrality, will filter Obtained active carbon saves in drier after 70 DEG C of drying 12h in drier, is denoted as 10%C6H8O7·H2O·GAC。 Fig. 2 is by the 10%C after citric acid-modified6H8O7·H2The SEM of OGAC schemes, it can be seen from the figure that the activity after being modified Carbon surface becomes coarse, and aperture becomes larger, and microcellular structure increased significantly, and gap is evenly distributed.
1 10%HNO of comparative example3·GAC
(1) Pre-Treatment of Activated charcoal: the step is identical as the pre-treatment step of active carbon in embodiment 1;
(2) modifying agent is prepared, 65%~68% concentrated nitric acid for weighing 31.16ml is mixed with deionized water, configuration quality The HNO that concentration is 10%3Solution is denoted as 10%HNO3
(3) modified activated carbon
Active carbon in step (1) by pretreated 5.0g is immersed in 10% HNO prepared in step (2)3It is molten In liquid, active carbon is taken out after heating 2h in 75 DEG C of water-baths, the pH value by deionized water repeated flushing to flushing liquor is neutrality After filter, obtained active carbon will be filtered and be placed in drier, save, be denoted as in drier after 70 DEG C of drying 12h 10%HNO3·GAC.Fig. 3 is 10%HNO3The SEM of GAC schemes, it can be seen from the figure that relative to unmodified active carbon, quilt HNO3Modified active carbon, microcellular structure increase, but the density of micropore is not so good as in embodiment 1 by the activity after citric acid-modified Charcoal.
2 10%NaOHGAC of comparative example
(1) Pre-Treatment of Activated charcoal: the step is identical as the pre-treatment step of active carbon in embodiment 1;
(2) modifying agent is prepared, the NaOH solid for weighing 11.2g is mixed with deionized water, and configuration quality concentration is 10% NaOH solution is denoted as 10%NaOH.
(3) modified activated carbon
It is molten that active carbon in step (1) by pretreated 5.0g is immersed in 10% NaOH prepared in step (2) It in liquid, takes out after impregnating 2h, by the pH value of deionized water repeated flushing to flushing liquor to be filtered after neutrality, suction filtration is obtained Active carbon is placed in drier, is saved in drier after 70 DEG C of drying for 24 hours, is denoted as 10%NaOHGAC.Fig. 4 is quilt The SEM of the modified active carbon of NaOH schemes, it can be seen from the figure that the hole for the active carbon being modified be not so good as by citric acid or HNO3Modified activated carbon surface is uniform, to be attached with aperture in macropore.
Comparative example 3 prepares 10%KOHGAC
(1) Pre-Treatment of Activated charcoal: the step is identical as the pre-treatment step of active carbon in embodiment 1;
(2) modifying agent is prepared, the KOH solid for weighing 11.2g is mixed with deionized water, and configuration quality concentration is 10% KOH solution is denoted as 10%KOH.
(3) modified activated carbon
Active carbon in step (1) by pretreated 5.0g is immersed in 10% KOH solution prepared in step (2) In, it is taken out after impregnating 2h, by the pH value of deionized water repeated flushing to flushing liquor to be filtered after neutrality, the work that suction filtration is obtained Property charcoal in drier, saved in drier after 70 DEG C of drying for 24 hours, be denoted as 10%KOHGAC.Fig. 5 is to be modified by KOH The SEM of active carbon afterwards schemes, it can be seen from the figure that being improved by the surface porosity factor of the modified active carbon of KOH, but hole Hole quantity is not so good as by the pore quantity of the NaOH active carbon being modified.
Active carbon is made to Pb in waste water to verify2+Adsorption capacity, prepare Pb2+Solution weighs the lead acetate of 0.033g Solid, prepares 100mL, and concentration is the Pb of 100mg/L2+Solution (mother liquor).Mother liquor is diluted to 1mg/L, 2mg/L, 3mg/ respectively L, the sub- liquid of 4mg/L, 5mg/L.
The drafting of standard curve: with atomic absorption spectrophotometry degree flame method, being compared with blank reagent, 283.3nm wavelength, Slit is the absorbance that institute's gamete liquid in determination step (3) is distinguished at 1.0nm, draws standard curve.Using concentration X (mg/L) as Abscissa, absorbance A bs are ordinate, draw standard curve, the related data of standard curve is as shown in table 1 below, standard curve As shown in Figure 6.
1 standard curve related data of table
According to the standard curve and Fig. 6, Pb in absorbance and solution can be obtained2+Concentration relationship regression equation such as following formula (1) shown in:
Abs=0.0304X+0.00321, R2=0.9964 (1)
Wherein, Abs is absorbance, X Pb2+Concentration, mg/L.
Shown in the adsorbance calculation formula such as following formula (2) of lead ion:
qt=V (CBegin-CEnd)/W (2)
In formula: qtIt indicates t moment adsorbance (mg/g);
V indicates liquor capacity (L);
W indicates that activated carbon weight (g) is added;
CBeginIndicate Pb before adsorbing2+Concentration;
CEndIndicate the Pb of t moment2+Concentration;
Shown in the removal rate calculation formula such as following formula (3) of lead ion:
η=[(CBegin-CEnd)/CBegin] × 100% (3)
In formula: η indicates the removal rate of lead ion, %;
CBeginIndicate Pb before adsorbing2+Concentration;
CEndIndicate the Pb of t moment2+Concentration;
2g active carbon modified in the unmodified active carbon of 2g, embodiment 1, comparative example 1- comparative example 3 is placed in 10mL, concentration are to pass through atomic absorption spectrophotometry degree flame method and standard curve after standing 2 hours in 100mg/L lead ion solution The plumbum ion concentration of the different phase containing lead solution is measured, convolution (2) calculates the lead ion removing of the active carbon of different modifications Rate, concrete outcome are as shown in table 2 below.
The lead ion removal efficiency of 2 different activities charcoal of table, %
It is from upper table 2 it is found that most strong by the ability of lead ion in the removing solution of the active carbon after citric acid-modified, Adsorption of Lead Ion effect is best, and removal efficiency can reach 68.54%.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.

Claims (8)

1. a kind of preparation method for the modified activated carbon for handling Pb In Exhausted Water ion, which is characterized in that include the following steps, it will be pre- The active carbon of treated 5.0g is immersed in the citric acid solution that mass concentration is 10%, is taken out after immersion, is passed through deionization Water repeated flushing active carbon filters after neutrality to the pH value of flushing liquor, the active carbon drying that suction filtration is obtained, obtained after dry By the active carbon of citric acid-modified, for the modified activated carbon for handling Pb In Exhausted Water ion.
2. a kind of preparation method of modified activated carbon for handling Pb In Exhausted Water ion according to claim 1, feature exist In, pretreated active carbon preparation method the following steps are included: wash commercially available active carbon several times by deionized water, until There is lamination in active carbon and deionized water;Active carbon is taken out, after active carbon for the first time drying, crushes, be ground up, sieved, After the active carbon of sieving is cleaned with deionized water, second of drying of active carbon is taken out, pretreated active carbon is made.
3. a kind of preparation method of modified activated carbon for handling Pb In Exhausted Water ion according to claim 2, feature exist In active carbon is dry for the first time and second of dry drying temperature is 70 DEG C, and drying time is 12h.
4. a kind of preparation method of modified activated carbon for handling Pb In Exhausted Water ion according to claim 2, feature exist In the sieving standard of active carbon is 60 mesh.
5. a kind of preparation method of modified activated carbon for handling Pb In Exhausted Water ion according to claim 1, feature exist In active carbon selects apricot shell active carbon.
6. a kind of preparation method of modified activated carbon for handling Pb In Exhausted Water ion according to claim 1, feature exist In the preparation process of 10% citric acid solution is to mix 2.1042g lemon granulates with deionized water, prepares mass concentration For 10% citric acid solution.
7. a kind of preparation method of modified activated carbon for handling Pb In Exhausted Water ion according to claim 1, feature exist In soaking time of the active carbon in 10% citric acid solution is 4h.
8. a kind of preparation method of modified activated carbon for handling Pb In Exhausted Water ion according to claim 1, feature exist In the drying temperature of filtered active carbon is 70 DEG C, drying time 12h.
CN201811289212.0A 2018-10-31 2018-10-31 A kind of preparation method for the modified activated carbon handling Pb In Exhausted Water ion Pending CN109499543A (en)

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Publication number Priority date Publication date Assignee Title
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CN106552612A (en) * 2015-09-29 2017-04-05 云南民族大学 A kind of microwave improves the method that activity of bamboo charcoal increases absorption property
CN107080287A (en) * 2016-02-15 2017-08-22 上海烟草集团有限责任公司 A kind of activated carbon dipping method of modifying and application

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1626455A (en) * 2003-12-09 2005-06-15 煤炭科学研究总院北京煤化工研究分院 Active carbon for controlling pH value of clarified water to be raised, and preparation method
CN102941065A (en) * 2012-11-06 2013-02-27 中国科学院山西煤炭化学研究所 Carbon-based material adsorbent for removing heavy metals in waste water, its preparation method and application
CN106552612A (en) * 2015-09-29 2017-04-05 云南民族大学 A kind of microwave improves the method that activity of bamboo charcoal increases absorption property
CN107080287A (en) * 2016-02-15 2017-08-22 上海烟草集团有限责任公司 A kind of activated carbon dipping method of modifying and application

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