CN107970895A - A kind of preparation and application of the biological adsorption material of heavy metal cadmium - Google Patents
A kind of preparation and application of the biological adsorption material of heavy metal cadmium Download PDFInfo
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- CN107970895A CN107970895A CN201711352217.9A CN201711352217A CN107970895A CN 107970895 A CN107970895 A CN 107970895A CN 201711352217 A CN201711352217 A CN 201711352217A CN 107970895 A CN107970895 A CN 107970895A
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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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/3425—Regenerating or reactivating of sorbents or filter aids comprising organic materials
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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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/345—Regenerating or reactivating using a particular desorbing compound or mixture
- B01J20/3475—Regenerating or reactivating using a particular desorbing compound or mixture in the liquid phase
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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
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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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
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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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
- C02F2303/00—Specific treatment goals
- C02F2303/16—Regeneration of sorbents, filters
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- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
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- Environmental & Geological Engineering (AREA)
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Abstract
The present invention relates to a kind of preparation of biological adsorption material, for removing heavy metal cadmium in water removal；Under certain condition, using Semen sesami nigrum as raw material, by microwave radiation technology, melanin is extracted from Semen sesami nigrum.Black sesame melanin has natural black pigment（melanin）Typical infrared signature, contain virtue（It is miscellaneous）The substituted radical such as the structures such as ring, quinone and aromatic carboxylic, alkyl, phenolic hydroxyl group, amino；With preferably combining genotoxic potential cation（Mainly transition metal ions）Characteristic, can be used as a kind of biological adsorption agent adsorbing heavy metal in water cadmium, it is safe and efficient, the mechanism of action is simple and reliable, method is effective.It is an advantage of the invention that preparing biological adsorption agent by basic material of Semen sesami nigrum, its raw material is agricultural product, derives from a wealth of sources, is cheap, is environmental-friendly, and preparation method is simple, equipment requirement is low, easy to large-scale production.
Description
Technical field
The present invention relates to a kind of biological adsorption material, belong to technical field of heavy metal wastewater treatment, be specifically an a kind of huge sum of money
Belong to preparation method and the application of the biological adsorption material of cadmium.
Background technology
Currently, heavy metal pollution becomes the serious environmental problem that the whole world faces, in all pollution elements,
Cadmium becomes one of object of greatest concern so that mobility is big, toxicity is high.According to Agricultural Environmental Monitoring master station of the Ministry of Agriculture 1996~1998
The monitoring result in year, irrigating region cadmium pollution area is maximum, up to 3.85 ten thousand hm2, the 56.9% of heavy metals exceeding standard area is accounted for, irrigating region
The agricultural product cadmium exceeding standard rate of production is up to 10.2%.
Cadmium（cadium）It is one of industry and environmental contaminants, experimental animal contamination and the research of Human body package is shown,
Cadmium can produce serious poisonous effect.In the toxin mainly studied in the world today, cadmium occupies the 3rd, its toxic action has drawn
Play the extensive concern of domestic and foreign scholars.United Nations Environment Programme proposes 12 kinds of dangerous substances with global meaning, cadmium
It is listed in first place；Poisonous substance administration committee of the U.S.（ATSDR）It is classified as the 6th noxious material for jeopardizing human health, and by
International cancer research institution is determined as the lung cancer of the mankind and experimental animal and the confirmation carcinogenic substance of prostate cancer.China is from 20th century
Since the eighties, start to investigate the Health Impact of Environmental Cadmium Pollution, it turns out that, Chinese industrial cadmium
Pollution is mainly started from the early 1960s, being related to 11 provinces by the area of cadmium pollution（City）25 areas；Every year with Industry Waste
Gurry is discharged into the total amount of the cadmium in environment more than 680000Kg.After the nineties, the Chinese Health Impact to cadmium pollution
Investigation, result of study show that the health hazard of these crowds is even more serious compared with the 1980s.Crowd in the world
Cadmium environmental contamination exposure, occur mainly in Japan and China, other countries crowd Environmental Cadmium exposure either intensity, hold
Continuous time or population health damage are in relatively low level.
It is more for the processing method of cadmium wastewater at present, institute different according to form existing for the content of cadmium ion and cadmium
The processing method of use is also different.Currently used method has chemical method, physical-chemical process, 3 major class of bioanalysis.But these sides
Method is difficult to put into practical application often because cumbersome, generation secondary pollution, excessively high etc. reason of input cost.
A kind of novel absorption material of low cost, simple and easy to get, environmental-friendly is needed to be gone for heavy metal cadmium for this
Remove.
Semen sesami nigrum（Semen Sesami Nigrum）It is Pedaliaceae（Pedaliaceae）The black seeds of Sesamum, are in the world
One of major oil crops, there are a large amount of plantations in many countries in Asia, South America and Central America.China is sesame production
, because Sesame Seed Yield is occupied first of the world, thus there is the title of " sesame kingdom " in big country.Black sesame melanin has natural black pigment
（melanin）Typical infrared signature, belong to a kind of melanin（melanin）.The structure of black sesame melanin is with aromatic ring
And quinone（Or part heteroaromatic）The conjugated system formed is connected with each other, there is aliphatic group, carboxyl, phenolic hydroxyl group, amino on aromatic ring
Deng substituted radical, have and preferably combine genotoxic potential cation（Mainly transition metal ions）Characteristic.
CN103894401B discloses a kind of plant restoration method for administering cadmium lead arsenic combined contamination soil, and this method is chosen
Cadmium concentration type castor-oil plant kind, by cadmium concentration type castor-oil plant and ciliate desert-grass with the cadmium lead arsenic pollution of intercropping system plantation to neutral pH
Soil in, and periodically harvest maturation castor-oil plant；Harvest ripe castor-oil plant and ciliate desert-grass top is sent to exclusive place and concentrates and do
Harmless treatment.This method repairing efficiency is long, and plant final disposal process is usually to burn recycling heavy metal, not really
Removing heavy metals are removed from environment.
CN101367575B discloses one kind and carries out harmless biological to heavy metal wastewater thereby containing cadmium using phycomycete collaboration system
The method for producing hydrogen while adsorption treatment twice, being mainly characterized by for this method utilize frustule wall and bacterium cell membrane association
With quick adsorption cadmium, at the same using chlamydomonas heavy metal stress effect in its incubation element sulphur lack effect have it is similar it
The characteristics of place, allows chlamydomonas to produce hydrogen at the same time except cadmium, and further using clostridium butyricum come the life for chlamydomonas photosynthesis accumulation of fermenting
Object amount produces hydrogen again, and the equal immobilization processing of the bacterium used during inhaling cadmium production hydrogen, finally obtains cadmium concentration clean water up to standard
With a large amount of hydrogen.This method phycomycete limited source, process are difficult to control, while the phycomycete subsequent treatment for having adsorbed heavy metal cadmium is numerous
It is trivial, biosphere is easily accessible, forms the cumulative effect of heavy metal.
The biological adsorption material of heavy metal cadmium a kind of simple and easy to get, cheap, environmental-friendly is needed for this to meet
Industrial needs.
The content of the invention
Preparation method of the present invention is：Selection is clean, the Semen sesami nigrum of this season harvest is raw material, cleans drying, adds alkali
Property ethanol extractant, infiltrate Microwave Extraction melanin adsorbent finished product.
It is as follows that step is made in specific preparation.
（1）Pre-treatment：After Semen sesami nigrum decontamination, drying is cleaned, pulverizes and sieves 60 mesh, by solid-to-liquid ratio 1：20（m:v）Add
Enter the ethanol -5%Na that mass fraction is 60 ~ 80%2CO3Solution infiltrates 30min, then using micro-wave oven microwave 2 as extractant
Minute, precipitation is put only, takes the supernatant of black spare.
（2）Extractant recycles：It is distilled to recover ethanol extractant.
（3）Concentrate and purify：It is true in 60 DEG C after being filtered with distilled water flushing to neutrality by melanin extracting solution distillation and concentration
Sky is dry to constant weight, obtains adsorbent finished product.
The above-mentioned preparation-obtained product of preparation method has certain adsorption effect to heavy metal cadmium.
The concrete application method of the present invention：The cadmium-containing solution of 100mL 50mg/L is configured, adjustment cadmium-containing solution PH=4.0, add
Enter the adsorbent finished product of 0.20g, 3 h of constant temperature oscillation under the conditions of 25 DEG C, 120 r/min, centrifugal treating after reaction, with band
There is the filtering of filter needle tubing, the final cadmium content of its liquid containing cadmium reaction is detected with atomic absorption spectrophotometry.By formula（1）And formula（2）
Its adsorbance and adsorption rate are calculated respectively.
（Formula 1）.
（Formula 2）.
In formula, qe- adsorbance（mg/g）；η-adsorption rate（%）；V- cadmium-containing solution volumes（L）；C0- cadmium-containing solution it is initial dense
Degree（mg/L）；CeThe adsorption equilibrium concentration of-cadmium-containing solution（mg/L）；M- is sorbent used quality（g）.
Adsorbent desorbs：By the above-mentioned adsorbent for reaching equilibrium concentration, filtering drying is taken out, into the adsorbent being settled out
It is 1 to add solid-liquid ratio:10 0.02 mol/L disodium ethylene diamine tetraacetates (EDTA -2Na) solution, constant temperature oscillation 3
Centrifuged after h, take adsorbent to precipitate.Precipitation is washed till neutrality, is freeze-dried, up to the adsorbent after desorption and regeneration.
（3）.
In formula, Qi- desorption quantity（mg/g）；Q0- adsorbance（mg/g）；W- desorption efficiencies（%）.
The present invention includes following beneficial effect.
（1）The present invention prepares adsorbent with Semen sesami nigrum element for basic material, its raw material is agricultural product, is derived from a wealth of sources, price
It is cheap, environmental-friendly.And preparation method is simple, equipment requirement is low, easy to large-scale production.
（2）The present invention is using Semen sesami nigrum base material as raw material, by black by the use of ethanol as extractant, Microwave Extraction under alkaline condition
Melanin in sesame, functional group in melanin by chelation effectively and Cd2+Ion forms coordination, so as to fulfill pin
To the adsorption function of heavy metal cadmium, the mechanism of action is simple and reliable, and method is effective.
（3）Biomass adsorbent prepared by the present invention, regeneration desorption are simple.By adding chelating agent ethylenediamine tetra-acetic acid two
Sodium (EDTA -2Na), heavy metal is parsed, realizes adsorbent reactivation, and simple operation.
Embodiment
Embodiment 1.
By Semen sesami nigrum decontamination, clean be dried for standby, by solid-to-liquid ratio 1：20（To over dry raw material）It is 60% to add mass fraction
Ethanol -0.5%Na2CO3Solution, infiltrates 30min, is put into micro-wave oven and extracts 2 minutes, puts precipitation only after 30 minutes, filtering is stayed
Take black supernatant；Ethanol extractant is recovered by distillation, by melanin extracting solution distillation and concentration, with deionized water rinsing into
Property, after filtering, constant weight is dried under vacuum in 60 DEG C, obtains adsorbent finished product.The adsorbent is detected to Cd with cadmium wastewater2+Suction
Attached effect.Adjustment cadmium-containing solution temperature is 25 DEG C, PH=4, measures 100mL and is put into hard straight plastic tube, adds the above-mentioned suction of 0.2g
Attached dose of finished product, the isothermal vibration 3h on 25 DEG C, 120r/min oscillators, centrifugal treating after reaction, is filtered with filter needle tubing,
With the final cadmium content of its cadmium wastewater of aas determination, its adsorbance and adsorption rate are calculated respectively.It is computed adsorbing
Rate is 91.8%, adsorbance 22.95mg/g.
Reach the adsorbent of equilibrium concentration, take out filtering drying, it is 1 that solid-liquid ratio is added into the adsorbent being settled out:10
0.02mol/L disodium ethylene diamine tetraacetates（EDTA-2Na）Solution, centrifuges after constant temperature oscillation 3h, takes adsorbent to precipitate, will be heavy
Shallow lake is washed till neutrality, and freeze-drying, adds 100ml water to dilute, and the HCl solution of 0.5mol/L adjusts pH to 4, the constant temperature oscillation at 25 DEG C
3h is reacted, is stood, Aspirate supernatant filtering, measures Cd in solution2+Content, by formula calculate desorption efficiency be 70.1%.
Embodiment 2.
By Semen sesami nigrum decontamination, clean be dried for standby, by solid-to-liquid ratio 1：20（To over dry raw material）It is 70% to add mass fraction
Ethanol -5%Na2CO3Solution, infiltrates 30min, is put into micro-wave oven and extracts 2 minutes, puts precipitation only after 30 minutes, filtering is left and taken
Black supernatant；Ethanol extractant is recovered by distillation, by melanin extracting solution distillation and concentration, with deionized water rinsing into
Property, after filtering, constant weight is dried under vacuum in 60 DEG C, obtains adsorbent finished product.Add according to the identical step of example 1 and give up containing cadmium
Water, it is 93.2% to be computed adsorption rate, adsorbance 23.3mg/g, resolution factor 68.6%.
Embodiment 3.
By Semen sesami nigrum decontamination, clean be dried for standby, by solid-to-liquid ratio 1：20（To over dry raw material）It is 80% to add mass fraction
Ethanol -5%Na2CO3Solution, infiltrates 30min, is put into micro-wave oven and extracts 2 minutes, puts precipitation only after 30 minutes, filtering is left and taken
Black supernatant；Ethanol extractant is recovered by distillation, by melanin extracting solution distillation and concentration, with deionized water rinsing into
Property, after filtering, constant weight is dried under vacuum in 60 DEG C, obtains adsorbent finished product.Add according to the identical step of example 1 and give up containing cadmium
Water, it is 92.1% to be computed adsorption rate, adsorbance 23.03mg/g.Resolution factor is 69.2%.
Application example 1.
Under different cadmium wastewater concentration conditions, the adsorbent is to Cd2+Adsorption effect.Preparation cadmium content for 1ppm ~
The liquid containing cadmium reaction of 200ppm, it is 25 DEG C to adjust cadmium-containing solution temperature, PH=4, and measurement 100ml, which is put into hard straight plastic tube, to be added
Enter the adsorbent finished product in 0.02g embodiments 2.The isothermal vibration 3h on 25 DEG C, 120r/min oscillators, after reaction at centrifugation
Reason, is filtered with filter needle tubing, detects the final cadmium content of its cadmium wastewater with atomic absorption spectrophotometer method, calculate respectively
Its adsorbance and adsorption rate, are shown in Table 1.
Melanin is to Cd under the different cadmium wastewater concentration conditions of table 12+Adsorption effect
| C0 /ppm | Ce /ppm | η/% | q /mg/g |
| 1 | 0.068 | 93.22 | 0.47 |
| 5 | 0.397 | 92.06 | 2.30 |
| 10 | 0.830 | 91.70 | 4.56 |
| 20 | 1.690 | 91.55 | 9.16 |
| 50 | 4.270 | 91.46 | 22.87 |
| 100 | 8.940 | 91.06 | 45.53 |
| 200 | 37.080 | 81.46 | 81.46 |
Claims (3)
1. a kind of preparation method of the biological adsorption material of heavy metal cadmium, it is characterised in that comprising the following steps is：
（1）The preparation of adsorbent：Semen sesami nigrum decontamination is cleaned, is dried for standby, is pulverized and sieved（60 mesh）, adding mass fraction is
60% ~ 80% ethanol -5%Na2CO3Solution extractant, is 1 according to solid-liquid ratio：20（m:v）, after infiltrating 30 minutes, it is put into micro-wave oven
Middle extraction 2 minutes, after putting precipitation only, black supernatant is left and taken in filtering；It is recovered by distillation ethanol extractant, it is distillation and concentration, true
Up to melanin adsorbent finished product after sky is dry；
（2）The desorption of adsorbent：By the above-mentioned adsorbent for reaching equilibrium concentration, filtering drying is taken out, to the melanin being settled out
Middle addition solid-liquid ratio is 1:10 0.02 mol/L disodium ethylene diamine tetraacetates (EDTA -2Na) solution, constant temperature oscillation
Centrifuged after 3 h, take melanin deposition；Precipitation is washed till neutrality, is freeze-dried, up to the melanin adsorbent after desorption and regeneration
Finished product.
A kind of 2. biological adsorption material of heavy metal cadmium made from preparation method according to claim 1, it is characterised in that：
Ethanol-the 5%Na that it is 60 ~ 80% with mass fraction that adsorbent, which prepares optimal conditions to be,2CO3Solution is as extractant, solid-liquid ratio 1:
20, infiltrate 30 minutes, with microwave oven extraction 2 minutes.
3. the desorption of biological adsorption agent according to claim 1, it is characterised in that：With 0.02mol/L ethylenediamine tetra-acetic acids
Disodium (EDTA -2Na) solution, is 1 according to solid-liquid ratio:10 constant temperature oscillation 3h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112791710A (en) * | 2020-12-24 | 2021-05-14 | 天津工业大学 | Modified polymer fiber ball, preparation method thereof and Cd (II) polluted soil remediation method |
| CN117753372A (en) * | 2024-01-02 | 2024-03-26 | 中北大学 | Natural melanin hydrogel adsorption microsphere and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112791710A (en) * | 2020-12-24 | 2021-05-14 | 天津工业大学 | Modified polymer fiber ball, preparation method thereof and Cd (II) polluted soil remediation method |
| CN117753372A (en) * | 2024-01-02 | 2024-03-26 | 中北大学 | Natural melanin hydrogel adsorption microsphere and preparation method and application thereof |
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