CN105289562B - Heavy metal wastewater thereby recoverying and utilizing method - Google Patents
Heavy metal wastewater thereby recoverying and utilizing method Download PDFInfo
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- CN105289562B CN105289562B CN201510785994.7A CN201510785994A CN105289562B CN 105289562 B CN105289562 B CN 105289562B CN 201510785994 A CN201510785994 A CN 201510785994A CN 105289562 B CN105289562 B CN 105289562B
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Abstract
The invention discloses a kind of heavy metal wastewater thereby recoverying and utilizing methods.By molecular sieve and activated alumina in mass ratio 1:5 mixing, and vacuum saves after multiplicity reactivation at 140-160 DEG C；It puts into the waste water containing heavy metal, adjusts pH to 5~7 with sodium hydroxide, be stirred to react；The composite adsorbing material filter residue for having adsorbed heavy metal ion is impregnated in saturated sodium chloride solution, is stirred by filtrate direct emission, and filtering gained filtrate is heavy metal concentrate, and filter residue is washed with deionized, the composite adsorbing material after being desorbed；Drying obtains regenerated active composite adsorbing material and recycles；Na is added in heavy metal concentrate2S·9H2O recycles heavy metal.Compound using the 4A molecular sieve and 13X molecular sieve and activated alumina of industrialized production, activated alumina can both increase the specific surface area of molecular sieve, can also increase the intensity and thermal stability of molecular sieve, and recycling is convenient, reduces the loss of molecular sieve powder.
Description
Technical field
The invention belongs to water process and field of environment protection, are related to a kind of heavy metal wastewater thereby recoverying and utilizing method.
Background technique
With the rapid development of modern industry, problem of environmental pollution is increasingly severe, wherein heavy metal pollution is had become as people
Focus of attention.Heavy metal wastewater thereby is largely discharged into environment, cannot can only be occurred to migrate and be converted by natural degradation,
It is enriched with through biological chain, finally seriously threatens human health.
It is also just not identical to the pollution level of water body since the existing forms of heavy metal ion in water are different.According to
The processing of heavy metal wastewater thereby can be divided into physical removal and chemistry removal by the method for heavy-metal ion removal.Physical removal master
Include membrane separation process, evaporation concentration method etc., i.e., do not change the form of metal ion, passes through the method for concentration and separation removal.
Chemistry removal includes mainly chemical precipitation method, oxidation-reduction method, electrochemical process, iron oxidizing process and absorption method etc., i.e., by waste water
Metal ion is transformed into the method that insoluble substance is able to remove in system, and wherein chemical precipitation method is most widely used.
The method of common chemical precipitation is that a certain amount of flocculant and macromolecule flocculation aid are added into waste water.This chemical precipitation
Method has many advantages, such as that at low cost, simple, convenient management, effect are good.But the disadvantage is that sediment weight is big, sediment moisture content is high,
It is dehydrated relatively difficult, and this method choice is poor, therefore will increase sediment weight in actual waste water treatment process, easily produces
Raw secondary pollution.
Absorption method becomes the emphasis of research because material is cheap and easily-available, at low cost, removal effect is good, has researcher with tired support
Stone be modified absorbing heavy metal ions in water, there are also researcher directly adopt natural zeolite or with modified zeolite to heavy metal ion into
Row absorption, but the preparation of these materials and modifying process are often complicated cumbersome, and adsorption efficiency is not high enough.
For molecular sieve because its adsorption capacity is big, adsorption reaction is fast, and removal effect is good, becomes the green wood of processing heavy metal wastewater thereby
Expect, ion-exchange performance possessed by absorption property possessed by the biggish specific surface area of molecular sieve and tradable cation,
With the double effects of chemisorption and ion exchange in heavy metal containing wastewater treatment, there is important ground in field of waste water treatment
Position.But molecular sieve powder can be lost and damage during handling heavy metal wastewater thereby, and the rate of recovery is lower；Molecular sieve stability compared with
Difference, recycling activation effect are lower, and molecular sieve processing heavy metal wastewater thereby will also be become by, which recycling after heavy metal ion concentration, is badly in need of
It solves the problems, such as.
Summary of the invention
The purpose of the present invention is overcoming the prior art, a kind of method easy to operate, at low cost is provided, can be located
Heavy metal wastewater thereby is managed, and adsorbent material and heavy metal resourcesization can be utilized.
In order to achieve the above objectives, as follows using technical solution：
Heavy metal wastewater thereby recoverying and utilizing method, includes the following steps：
1) by molecular sieve and activated alumina in mass ratio 1:5 mixing, and vacuum is protected after multiplicity reactivation at 140-160 DEG C
It deposits；
2) composite adsorbing material after activation is put into the waste water containing heavy metal, with sodium hydroxide adjust pH to 5~
7, it is stirred to react, stands, filtering；
2) filtrate direct emission, filter residue are dry under the composite adsorbing material room temperature for having adsorbed heavy metal ion；
3) the composite adsorbing material filter residue for having adsorbed heavy metal ion impregnated in saturated sodium chloride solution, stirred, mistake
Filter gained filtrate is heavy metal concentrate, and filter residue is washed with deionized, the composite adsorbing material after being desorbed；
4) composite adsorbing material after desorption is dried to obtain regenerated active composite adsorbing material, is recycled for wastewater treatment
It utilizes；Na is added in heavy metal concentrate2S·9H2O solid powder generates sulfide precipitation, recycles heavy metal.
According to the above scheme, the molecular sieve is 4A molecular sieve or 13X molecular sieve.
According to the above scheme, the dosage of the composite adsorbing material is 0.5~1.5g/L.
According to the above scheme, step 1 composite adsorbing material, which is put into, is stirred to react 10~60min in the waste water containing heavy metal,
Stand 10~30min.
According to the above scheme, the heavy metal is Pb2+、Cd2+、Cu2+、Ni2+Equal cations, concentration are 20~400mg/L.
According to the above scheme, the dosage of saturated sodium chloride solution described in step 3 is the 1/5 of the heavy metal wastewater thereby volume,
Mass concentration is 26.5%.
According to the above scheme, the composite adsorbing material drying temperature after step 4 desorption is 100~110 DEG C, and the time is 2~3h.
The present invention handles heavy metal wastewater thereby and recycles and has the beneficial effect that using molecular sieve：
Compound with activated alumina using the 4A molecular sieve and 13X molecular sieve of industrialized production, activated alumina both may be used
To increase the specific surface area of molecular sieve, the intensity and thermal stability of molecular sieve can also be increased, recycling is convenient, reduces molecular sieve powder
The loss at end.By the effect of absorption-ion exchange, by the removal of heavy metal ions in waste water, dosage is small, reaction efficiency
Height, saturated adsorption capacity reach 200~500mg/g.
Molecular sieve after being desorbed with saturated sodium chloride solution can regenerate, and can be recycled, and concentrate is through being added Na2S·
9H2O solid powder generates sulfide precipitation, and heavy metal can be recycled.
Small investment, at low cost, processing waste water is high-efficient, easy to operate, without secondary pollution, can obtain and be applicable.
Specific embodiment
Following embodiment further illustrates technology contents of the invention, but not as limiting the scope of the invention.
Embodiment 1：
(1) at 25 DEG C of room temperature, with commercially available 4A molecular sieve and activated alumina, Hybrid Heating production is compound at 150 DEG C
Adsorbent material prepares the waste water containing Pb that initial concentration is 50mg/L, and adjusting initial pH on wastewater value is 5, and molecular sieve dosage is
0.5g/L, and being sufficiently mixed, stirs 50 minutes under the action of six blenders, and 200 revs/min of mixing speed, stratification
30min, it is 95.06% that treated waste water plumbum ion concentration, which is 2.47mg/L removal rate,.
(2) the leaded composite adsorbing material of recycling is dried and is saved, prepare a certain amount of saturated sodium chloride solution, washing is stirred
Mix 10-15min, finally use distilled water flushing, using it is a small amount of it is multiple by the way of, the body of saturated sodium chloride solution and heavy metal wastewater thereby
Product is than about 1:5.The composite adsorbing material of recycling is placed in drying box and dries 2-3h at 100 DEG C, after obtaining activation after cooling
4A molecular sieve and active aluminum oxide composite adsorbing material.
(3) it is desorbed by saturated sodium chloride solution, plumbum ion concentration is 235.6mg/L in concentrate, and cycles of concentration is
4.7.The 4A molecular sieve removal rate 92.3% of secondary use, the removal rate after four recyclings are 86.7%.
Embodiment 2：
At 25 DEG C of room temperature, with commercially available 4A and 13X molecular sieve and activated alumina, Hybrid Heating production is multiple at 150 DEG C
Adsorbent material is closed, CdCl is used2The waste water containing Cd that initial concentration is 100mg/L is prepared, adjusting initial pH on wastewater value is 7, compound suction
The dosage of enclosure material is 1.5g/L, and is sufficiently mixed, and is stirred 50 minutes under the action of six blenders, mixing speed 200
Rev/min, the waste water concentration of cadmium ions after stratification 30min, 4A molecular sieve combined processing is 1.5mg/L, and removal rate reaches
98.5%；Waste water concentration of cadmium ions after 13X molecular sieve combined processing is 1.2mg/L, and removal rate reaches 98.8%.
Embodiment 3：
At room temperature at 25 DEG C, with commercially available 13X molecular sieve and activated alumina, Hybrid Heating production is compound at 150 DEG C
Adsorbent material prepares the chromate waste water that 400mL concentration is 20mg/L with chromium chloride, and adjusting initial pH on wastewater value is 5, composite adsorption
Material dosage is 1.0g/L, and is sufficiently mixed, and is stirred 50 minutes under the action of six blenders, 200 turns of mixing speed/
Point, stratification 30min takes supernatant.Treated that waste water chromium ion removal rate has reached 92.2% for composite adsorbing material.
Embodiment 4：
At room temperature at 25 DEG C, with commercially available 4A molecular sieve and activated alumina, Hybrid Heating production is compound at 150 DEG C
Adsorbent material prepares the copper-containing wastewater that 400mL concentration is 400mg/L with copper chloride, and adjusting initial pH on wastewater value is 5, compound suction
Enclosure material dosage is 1.5g/L, and is sufficiently mixed, and is stirred 50 minutes under the action of six blenders, 200 turns of mixing speed/
Point, stratification 30min takes supernatant.Treated that waste water copper ion removal rate has reached 96.8% for composite adsorbing material.
Embodiment 5：
At room temperature at 25 DEG C, mixed at 150 DEG C with commercially available 4A molecular sieve and 13X molecular sieve with activated alumina plus
Heat production composite adsorbing material, prepares the copper-containing wastewater that 400mL concentration is 200mg/L with copper chloride, adjusts initial pH on wastewater value
It is 7, composite adsorbing material dosage is 1.5g/L, and is sufficiently mixed, and is stirred 50 minutes under the action of six blenders, is stirred
200 revs/min of speed, stratification 30min takes supernatant.Treated that waste water copper ion removal rate reaches for composite adsorbing material
99.2%.
Claims (5)
1. heavy metal wastewater thereby recoverying and utilizing method, it is characterised in that include the following steps：
1) by molecular sieve and activated alumina in mass ratio 1:5 mixing, and vacuum saves after multiplicity reactivation at 140-160 DEG C；
The molecular sieve is 4A molecular sieve or 13X molecular sieve；
2) composite adsorbing material after activation is put into the waste water containing heavy metal, adjusts pH to 5~7 with sodium hydroxide, stirs
Reaction is mixed, is stood, filtering；
2) filtrate direct emission, filter residue are dry under the composite adsorbing material room temperature for having adsorbed heavy metal ion；
3) the composite adsorbing material filter residue for having adsorbed heavy metal ion impregnated in saturated sodium chloride solution, stirred, filter institute
Obtaining filtrate is heavy metal concentrate, and filter residue is washed with deionized, the composite adsorbing material after being desorbed；
4) composite adsorbing material after desorption is dried to obtain regenerated active composite adsorbing material, recycles benefit for wastewater treatment
With；Na is added in heavy metal concentrate2S·9H2O solid powder generates sulfide precipitation, recycles heavy metal；The compound suction
Enclosure material drying temperature is 100~110 DEG C, and the time is 2~3h.
2. heavy metal wastewater thereby recoverying and utilizing method as described in claim 1, it is characterised in that the throwing of the composite adsorbing material
Dosage is 0.5~1.5g/L.
3. heavy metal wastewater thereby recoverying and utilizing method as described in claim 1, it is characterised in that the composite adsorbing material after activation is thrown
Enter and be stirred to react 10~60min into the waste water containing heavy metal, stands 10~30min.
4. heavy metal wastewater thereby recoverying and utilizing method as described in claim 1, it is characterised in that the heavy metal is Pb2+、Cd2+、
Cu2+Or Ni2+, concentration is 20~400mg/L.
5. heavy metal wastewater thereby recoverying and utilizing method as described in claim 1, it is characterised in that saturated sodium-chloride described in step 3 is molten
The dosage of liquid is the 1/5 of the heavy metal wastewater thereby volume, mass concentration 26.5%.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108585097B (en) * | 2018-02-13 | 2021-03-26 | 洛阳理工学院 | Adsorption treatment method for copper ion-containing wastewater |
| CN108585103A (en) * | 2018-05-16 | 2018-09-28 | 暨南大学 | A method of absorption and thermostabilization heavy metal from low-concentration heavy metal boiling water |
| CN111921496A (en) * | 2020-07-10 | 2020-11-13 | 广东石油化工学院 | Composite adsorbent and preparation method and application thereof |
| CN112495342B (en) * | 2020-11-04 | 2022-01-04 | 大连理工大学 | Method for removing cadmium ions in water by using defective MFI molecular sieve as adsorbent |
| CN112321104A (en) * | 2020-11-27 | 2021-02-05 | 北京嘉盛天合气体科技有限公司 | River and lake bottom mud curing repairing agent and preparation method thereof |
| CN114288986A (en) * | 2021-08-20 | 2022-04-08 | 天津市万鑫众达科技发展有限公司 | Formula and production method of special adsorbent for radon and radon daughter aerosol |
| CN115521012A (en) * | 2022-10-08 | 2022-12-27 | 合肥中科弘逸环保科技有限责任公司 | Method for treating in-situ synthesized Cu-SSZ-13 molecular sieve waste liquid |
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| CN1359749A (en) * | 2000-12-08 | 2002-07-24 | 环球油品公司 | Composite adsorbent for purifying hydrocarbon stream |
| CN102689938A (en) * | 2012-05-23 | 2012-09-26 | 北京佳康尔水处理技术有限公司 | 13x molecular sieve water purifying device for purifying heavy metal in drinking water |
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| CN101007261B (en) * | 2006-12-17 | 2010-05-12 | 于向真 | Zeolite adsorbent and its preparation method |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1359749A (en) * | 2000-12-08 | 2002-07-24 | 环球油品公司 | Composite adsorbent for purifying hydrocarbon stream |
| CN102689938A (en) * | 2012-05-23 | 2012-09-26 | 北京佳康尔水处理技术有限公司 | 13x molecular sieve water purifying device for purifying heavy metal in drinking water |
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