CN108085012A - It is a kind of for passivator of Cd contaminated soils and preparation method thereof - Google Patents
It is a kind of for passivator of Cd contaminated soils and preparation method thereof Download PDFInfo
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- CN108085012A CN108085012A CN201711385414.0A CN201711385414A CN108085012A CN 108085012 A CN108085012 A CN 108085012A CN 201711385414 A CN201711385414 A CN 201711385414A CN 108085012 A CN108085012 A CN 108085012A
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- charcoal
- passivator
- sulfhydryl modified
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- humic acid
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K17/00—Soil-conditioning materials or soil-stabilising materials
- C09K17/40—Soil-conditioning materials or soil-stabilising materials containing mixtures of inorganic and organic compounds
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
- C05G3/80—Soil conditioners
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2101/00—Agricultural use
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Soil Sciences (AREA)
- Organic Chemistry (AREA)
- Pest Control & Pesticides (AREA)
- Inorganic Chemistry (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Processing Of Solid Wastes (AREA)
- Soil Conditioners And Soil-Stabilizing Materials (AREA)
Abstract
The invention discloses a kind of for passivator of Cd contaminated soils and preparation method thereof.The passivator is made of sulfhydryl modified charcoal, zeolite powder and humic acid；The mass ratio of the sulfhydryl modified charcoal, the zeolite powder and the humic acid is 45~55：35~45：5~15；The sulfhydryl modified charcoal is obtained by the reaction by charcoal and sulfhydryl compound.The present invention by by charcoal carry out it is sulfhydryl modified after, and zeolite, humic acid rational proportion, mixing granulation, obtained passivator is fast to heavy metal adsorption rate, adsorption effect, stablize it is lasting.Charcoal after sulfhydryl modified enhances the affinity of heavy metal Cd, improves the adsorption efficiency and stability to heavy metal Cd；Sulfydryl charcoal and zeolite rational proportion, synergistic effect is played to the passivation of heavy metal Cd；Humic acid and Cd2+Easily combine but and it is unstable, can be used as transfer from Cd2+Medium carrier adsorb cadmium in soil with promoting sulfydryl charcoal and zeolite fast and stable.
Description
Technical field
The present invention relates to a kind of for passivator of Cd contaminated soils and preparation method thereof, belong to soil restoring technology neck
Domain.
Background technology
In recent years, soil pollution by heavy metal problem getting worse.It is announced according to national environmental protection portion and Ministry of Land and Resources
's《National Soil Pollution Investigation publication in 2014》It has been shown that, the national total exceeding standard rate of soil reach 16.1%, arable soil point
Position exceeding standard rate reaches 19.4%.One of cadmium heavy metal element most strong as toxicity influences the physiology of crop by contaminated soil
Metabolism, and then human health is influenced by the enrichment of food chain.The reparation of heavy-metal contaminated soil is a generally acknowledged problem, mesh
Though the preceding report for having the technical measures such as physics, biology, chemistry and agronomy, there are still quantities is big, expense in practical applications
The expensive, shortcomings such as repair time is long, governance efficiency is low.For the repairing and treating in the farmland of cadmium pollution, in-situ passivation technology is fortune
Heavy metal is converted into the inactive form of chemical property with method physically or chemically, by reducing crop to a huge sum of money in soil
Belong to the transfer and enrichment of cadmium, the risk of human health is endangered so as to reduce heavy metal by food chain, be a kind of more economical feasible
Technical method.But at present applied to Cd-polluted farmland passivator there are it is of high cost, passivation efficiency is low, passivation effect not
The shortcomings of stablizing limits the further genralrlization of the technology.
In recent years, China has carried out the technical research that some charcoals are passivated heavy metal-polluted soil Cd, such as Publication No.
The Chinese invention patent application of CN102807872A provide a kind of raw material for charcoal, medical stone powder, diatomite in powder, lignite and
The soil heavy mental adsorbent of flyash；The Chinese invention patent application of Publication No. CN103740373A provides a kind of by life
Object charcoal, calcined shell and the mixed stabilization agent of bone meal are applied to the soil of heavy metal pollution；Publication No.
The Chinese invention patent application of CN105967940A provides a kind of iron-based life that can be applied to administer arsenic cadmium combined pollution soil
Object Carbon Materials.But existing heavy metal deactivator is weaker to the heavy metal especially affinity of Cd, therefore during presence balance
Between it is long, passivation efficiency is low, stability is poor the problem of.To sum up, it is desirable to provide it is a kind of it is short to heavy metal especially Cd equilibration times,
The strong passivator of advantages of good adsorption effect, stability.
The content of the invention
The object of the present invention is to provide a kind of passivator for Cd contaminated soils, and the passivator is to heavy metal especially Cd
The rate of adsorption is fast, good passivation effect, stablize it is lasting；And the raw material sources that prepare the passivator are extensive, it is of low cost, prepare
Method is simple and suitable mechanization application.
Passivator of the present invention in biological carbon surface by introducing substantial amounts of active group-sulfydryl, by between sulfydryl and Cd
Coordination improve passivator to the adsorption capacity of Cd；Clay mineral and humic acid also have stronger absorption property to Cd,
It is used cooperatively with charcoal and synergistic effect is played to the heavy metal especially passivation of Cd；Humic acid as in passivating process from
Sub- transfer vector, makes Cd2+It is quickly quietly adsorbed by sulfydryl charcoal and clay mineral.
Specifically, the technical solution of the passivator of heavy-metal contaminated soil provided by the invention is as follows：
The passivator is made of sulfhydryl modified charcoal, zeolite powder and humic acid.
Wherein, the mass ratio of the sulfhydryl modified charcoal, the zeolite powder and the humic acid can be 45~55：35~
45：10, concretely 50：40：10.
The grain diameter of the passivator can be 2~4mm, and hardness is more than 9N；
The mesh number of the sulfhydryl modified charcoal is more than 200 mesh, and pH is 7.0~10.0, and specific surface area is not less than 500m2/
G, sulfhydryl content are 2~3mmol/g；
The mesh number of the zeolite powder is not less than 200 mesh；
The pH of the humic acid is 4.0~6.0, organic matter (in terms of butt) >=80.0%, humic acid (butt) >=
60.0%.
The sulfhydryl modified charcoal can be obtained by the reaction by charcoal and sulfhydryl compound；
The specific surface area of the charcoal is not less than 200m2/ g, pH be 9~10, carbon content be 900~950g/kg, mesh number
Not less than 200 mesh.
The sulfhydryl compound can be thioacetic acid.
The sulfhydryl modified charcoal can be prepared according to the method included the following steps：
It activates the charcoal and obtains activation charcoal；In acid condition, it is the activation charcoal and sulfhydrylation is molten
Liquid mixes, reacted up to the sulfhydryl modified charcoal；
The mass volume ratio of the activation charcoal and the sulfhydrylation solution is 1g：1mL~3mL, concretely 1g：
2mL；
The temperature of the reaction can be 60 DEG C~100 DEG C, and the time can be 6h~10h, such as react 8h at 80 DEG C；
The sulfhydrylation solution is thioacetic acid and the mixed liquor of acetic anhydride.
In the mixed liquor, the volume ratio of the thioacetic acid and the acetic anhydride can be 9~11：7, concretely 10：
7；
In the mixed liquor, the concentration of the thioacetic acid can be 6~8mol/L；
The acidity of concentrated sulfuric acid adjustment and control system can be added in, is added in the sulfhydrylation solution as described in 1L as described in 0.1ml~0.5ml
The concentrated sulfuric acid.
Specifically, the charcoal can be activated in salpeter solution, such as in 0.01mol/L HNO3In solution；
It is described to further include drying after reaction, be ground up, sieved in the above-mentioned method for preparing the sulfhydryl modified charcoal
The step of, it after being filtered by vacuum, and washes with water 2~3 times, is ground up, sieved after 30 DEG C~40 DEG C dryings.
Invention further provides the preparation methods of the passivator, include the following steps：
The sulfhydryl modified charcoal, the zeolite powder and the humic acid are mixed into obtain mixture；The mixture warp
Graininess is granulated to obtain, through being drying to obtain the passivator；
Granulating disc can be used to be granulated；
In the granulation process into the mixture spray water, be in granular form it, obtained after drying granular blunt
Agent；
The amount of the water can be the 10~15% of the mixture quality.
In passivator of the present invention, sulfhydryl compound can be acted on by pi bond and adsorbed in biological carbon surface, and charcoal is carried out
It is mercapto-functionalized.The combination principle of sulfydryl and Cd is：From the angle analysis of inorganic chemistry, Cd2+The d rails that outer shell electron distribution is had time
Road is easily accepted by the lone pair electrons of sulphur atom, and the two can be coordinated bonding, form the complex of stereochemical structure；From the angle of organic chemistry
Degree analysis, interacts to form chemical bond, forms stable complexing between sulfydryl and heavy metal ion there is Lewis Acids and Bases
Object or crosslinking net chelate.Therefore by charcoal carry out it is mercapto-functionalized after, enhance charcoal to Cd2+Affinity, carry
It is high to Cd in soil2+Selectivity and absorption stability.
In passivator of the present invention, zeolite surface carries negative electrical charge, has layer structure, larger porosity and specific surface
Product, can be by Electrostatic Absorption, ion exchange and chemisorbed, by Cd2+It is fixed in interlayer lattice.Match somebody with somebody with sulfydryl charcoal and apply
When, zeolite can adsorb the precipitations such as the cadmium phosphate of charcoal Surface Creation, cadmium carbonate, release obstruction of the precipitation to charcoal hole
With the inhibitory action to charcoal surface group, the rate of adsorption and stability of the charcoal to heavy metal are enhanced.
In passivator of the present invention, humic acid is a kind of negatively charged bulky grain colloid, contains substantial amounts of phenolic hydroxyl group, carbonyl
Exchange adsorption, complexing, but its adsorption effect and shakiness can occur with heavy metal ion for the functional groups such as base, amido, carboxyl
It is fixed.It is used cooperatively with sulfydryl charcoal and zeolite, the heavy metal ion of absorption is transferred to sulfydryl by humic acid as medium carrier
On charcoal and clay mineral, sulfydryl charcoal and clay mineral and the contact probability of heavy metal ion are added, so as to accelerate
The rate of adsorption of the passivator to heavy metal；Humic acid has colloidal nature simultaneously, can be played in granulation process and bond and increase
Add the effect of granule strength.
To sum up, the present invention by by charcoal carry out it is sulfhydryl modified after, and zeolite, humic acid rational proportion, mixing granulation,
Obtained passivator is fast to heavy metal adsorption rate, adsorption effect, stablize it is lasting.Charcoal after sulfhydryl modified is to heavy metal Cd
Affinity enhancing, improve the adsorption efficiency and stability to heavy metal Cd；Sulfydryl charcoal and zeolite rational proportion, counterweight
The passivation of metal Cd plays synergistic effect；Humic acid and Cd2+Easily combine but and it is unstable, can be used as transfer from Cd2+Jie
Matter carrier adsorbs the cadmium in soil with promoting sulfydryl charcoal and zeolite fast and stable.
The present invention has the advantages that：
(1) soil heavy metal passivant obtained using raw materials such as sulfhydryl modified charcoal, zeolite powder and humic acid, formula
When rationally, applied to heavy metal Cd contaminated soil, equilibration time is short, and remediation efficiency is high, and stability is strong.
(2) passivator is graininess in the present invention, can combine rotary tillage ferti machine and apply farmland, be suitble to mechanization application, keep away
Exempt from manually to spread fertilizer over the fields and airborne dust endangers.
(3) humic acid is added in passivator of the present invention, heavy metal pollution of soil reparation is combined with increasing soil fertility.
Soil physico-chemical property can be improved, increase the gas permeability of soil, promote absorption of the plant to fertilizer such as N P and Ks, increase crop yield.
Description of the drawings
Fig. 1 is the influence of matal deactivator of the present invention and each component to Cadmium in Soil bio-available Zn concentration.
Specific embodiment
Experimental method used in following embodiments is conventional method unless otherwise specified.
The materials, reagents and the like used in the following examples is commercially available unless otherwise specified.
The preparation and analysis of embodiment 1, sulfydryl charcoal
The physical and chemical parameter for the charcoal that the present embodiment uses is as follows：
Specific surface area is 295m2/ g, pH 10, mesh number are 200 mesh.
The preparation method of sulfydryl charcoal：1. prepare activation charcoal (AC)：Charcoal is placed in 0.01mol/L HNO3
In solution after magnetic agitation 72h, cleaned 2~3 times with distilled water, 105 DEG C drying to constant weight to get activation charcoal；2. it prepares
Sulfhydrylation solution (SH)：It is thioacetic acid according to volume ratio：Acetic anhydride=10：7 and 1 ‰ concentrated sulfuric acid mixings, obtain sulfydryl solution,
Wherein, thioacetic acid is the chemically pure reagent of Chinese medicines group；3. according to AC：SH=1：2(kg：L ratio) is abundant by AC and SH
Mixing after sealing, is placed in 80 DEG C of reaction 8h in thermostatic control oscillator vibration.Finally mixture is taken out, be filtered by vacuum, and with distill
It is ground after water is dry at cleaning 2~3 times, 60~80 DEG C, crosses 100 mesh sieves, sulfydryl charcoal (SH-AC) is made.
Shown in the esterification such as formula (1) occurred during above-mentioned activated carbon is sulfhydryl modified, it is known that, it reacts in acid condition
Lower progress, the hydroxyl on activated carbon are sulfhydryl modified key reaction site.
The analysis of sulfydryl charcoal：It takes the above method that sulfhydryl modified charcoal is prepared, uses elemental analyser (CHN-
O-Rapid, Heraeus, Germany) measure element sulphur.Elemental analysis shows that this method introduces 2.30mmol/g on the activated carbon
Sulfydryl, these sulfydryls serve as most important activated adoption site in sulfhydryl modified charcoal absorption heavy metal especially Cd.
The mesh number of sulfydryl charcoal manufactured in the present embodiment is 200 mesh, and pH is that the scope of 9.8-sulfydryl charcoal is 7.0
~10.0, specific surface area 510m2/g。
The preparation of embodiment 2, heavy metal deactivator
50 parts of sulfhydryl modified charcoal, 40 parts of zeolite powder (mesh number is 200 mesh), 10 parts of humic acid prepared by embodiment 1,
It is mass parts, mixes to obtain mixture, then be granulated with granulating disc, granulation process is sprayed according to the 12% of mixture quality
Watering point, is in granular form it, passivator particle, grain size 2mm, hardness 9N is obtained after drying.
Embodiment 3, the potted plant experiment to cadmium pollution soil reparation
Heavy metal deactivator prepared by embodiment 2 is added to 3% mass fraction in cadmium pollution soil, the cadmium pollution
Soil is Xiangtan, Hunan Province somewhere agricultural land soil, and the total cadmium of the soil is 0.96mg/kg, and effective cadmium is 0.27mg/kg.Abundant mixing
Afterwards, it is 40%~50% to control moisture content, is digestion agent with EDTA-2Na after balancing 3 days, 7 days and 15 days respectively, and extraction is effective
State heavy metal is measured using Inductively coupled plasma mass spectrometry (ICP-MS).
Experimental result shows, balance and stability after 3 days, 7 days and 15 days effective cadmium content of soil fall to 76.8% respectively,
79.7% and 80.0%, it is seen that heavy metal deactivator of the present invention can effectively reduce available Cd in actual physical prospecting soil, and repair
Multiple efficiency is fast, and remediation efficiency is high.
Embodiment 4, heavy metal deactivator and its each one pack system compare cadmium pollution soil passivation effect
Xiangtan, Hunan Province Cd-polluted farmland soil (total cadmium is 0.96mg/kg, and effective cadmium is 0.27mg/kg) is taken, per basin 1kg
Soil.Charcoal, sulfydryl charcoal, zeolite, heavy metal deactivator (embodiment 2 are added respectively according to 3% dosage per basin soil
Prepare) and abundant mixing, the soil of passivator or its single component material is not added with as control (CK), controls the soil moisture content to be
50%, balance extracts soil available cadmium after 15 days.Soil available Cd is extracted with EDTA-2Na, using inductive coupling etc.
Ion mass-spectrometer (ICP-MS) measures.
Experimental result applies soil available Cd content after sulfhydryl modified charcoal as shown in Figure 1, compared with charcoal
It significantly reduces, reduces 20.31%；After applying passivator, soil available Cd content substantially less than singly applies zeolite, sulfydryl life
Object charcoal illustrates that heavy metal deactivator of the present invention is substantially better than the passivation ability of heavy metal each one pack system, and each group divides it
Between exist synergistic effect.
Claims (10)
1. a kind of passivator of heavy-metal contaminated soil, it is characterised in that：The passivator is by sulfhydryl modified charcoal, zeolite powder
It is made with humic acid.
2. passivator according to claim 1, it is characterised in that：The sulfhydryl modified charcoal, the zeolite powder and institute
The mass ratio for stating humic acid is 45~55：35~45：5~15；
The grain diameter of the passivator is 2~4mm, and hardness is more than 9N；
The mesh number of the sulfhydryl modified charcoal is more than 200 mesh, and pH is 7.0~10.0, and specific surface area is not less than 500m2/ g, sulfydryl
Content is 2~3mmol/g；
The mesh number of the zeolite powder is not less than 200 mesh.
3. passivator according to claim 1 or 2, it is characterised in that：The sulfhydryl modified charcoal is by charcoal and mercapto
Based compound is obtained by the reaction；
The specific surface area of the charcoal is not less than 200m2/ g, pH are 9~10, and carbon content is 900~950g/kg, and mesh number is not small
In 200 mesh.
4. passivator according to claim 3, it is characterised in that：The sulfhydryl compound is thioacetic acid.
5. the passivator according to claim 3 or 4, it is characterised in that：The sulfhydryl modified life is prepared as steps described below
Object charcoal：
It activates the charcoal and obtains activation charcoal；In acid condition, the activation charcoal is mixed with sulfhydrylation solution
It closes, it is reacted up to the sulfhydryl modified charcoal；
The sulfhydrylation solution is thioacetic acid and the mixed liquor of acetic anhydride.
6. passivator according to claim 5, it is characterised in that：The charcoal is activated in salpeter solution；
The temperature of the reaction is 60 DEG C~100 DEG C, and the time is 6h~10h；
Described the step of further including drying after reaction, being ground up, sieved.
7. the preparation method of passivator, includes the following steps any one of claim 1-6：By the sulfhydryl modified biology
Charcoal, the zeolite powder and the humic acid mix to obtain mixture；The mixture is described through being drying to obtain through being granulated to obtain graininess
Passivator.
8. preparation method according to claim 7, it is characterised in that：It is sprayed in the granulation process into the mixture
Water；
The amount of the water is the 10~15% of the mixture quality.
9. application of the passivator any one of claim 1-6 in Heavy Metals in Contaminated Soils is passivated.
10. application according to claim 9, it is characterised in that：The heavy metal is cadmium.
Priority Applications (1)
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Cited By (7)
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| CN108906872A (en) * | 2018-06-05 | 2018-11-30 | 杭州电子科技大学 | The method for administering waste water and heavy metal pollution of soil with calcining oyster shell powder |
| CN109675522A (en) * | 2019-01-31 | 2019-04-26 | 中国农业科学院农业环境与可持续发展研究所 | A kind of high-performance consolidates the preparation method and application of Cd biomass carbon |
| CN109913231A (en) * | 2019-04-18 | 2019-06-21 | 江西师范大学 | A kind of novel inorganic-biological carbon soil passivator and preparation method thereof |
| CN110028974A (en) * | 2019-05-09 | 2019-07-19 | 湖南联和环保科技有限公司 | A kind of heavy metal cadmium soil remediation passivator, preparation method and applications |
| CN110346444A (en) * | 2019-07-03 | 2019-10-18 | 河南农业大学 | The extracting method of heavy metal available state in a kind of yellow moist soil |
| CN115722185A (en) * | 2022-11-10 | 2023-03-03 | 贵州师范大学 | Sulfydryl-iron-based composite modified bentonite for cadmium removal and preparation method thereof |
| CN116870874A (en) * | 2023-09-07 | 2023-10-13 | 南昌航空大学 | Mercapto modified coffee grounds adsorbent, and preparation method and application thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108906872A (en) * | 2018-06-05 | 2018-11-30 | 杭州电子科技大学 | The method for administering waste water and heavy metal pollution of soil with calcining oyster shell powder |
| CN109675522A (en) * | 2019-01-31 | 2019-04-26 | 中国农业科学院农业环境与可持续发展研究所 | A kind of high-performance consolidates the preparation method and application of Cd biomass carbon |
| CN109913231A (en) * | 2019-04-18 | 2019-06-21 | 江西师范大学 | A kind of novel inorganic-biological carbon soil passivator and preparation method thereof |
| CN110028974A (en) * | 2019-05-09 | 2019-07-19 | 湖南联和环保科技有限公司 | A kind of heavy metal cadmium soil remediation passivator, preparation method and applications |
| CN110346444A (en) * | 2019-07-03 | 2019-10-18 | 河南农业大学 | The extracting method of heavy metal available state in a kind of yellow moist soil |
| CN115722185A (en) * | 2022-11-10 | 2023-03-03 | 贵州师范大学 | Sulfydryl-iron-based composite modified bentonite for cadmium removal and preparation method thereof |
| CN116870874A (en) * | 2023-09-07 | 2023-10-13 | 南昌航空大学 | Mercapto modified coffee grounds adsorbent, and preparation method and application thereof |
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