CN106367076B - The preparation method of organic-inorganic compoiste heavy-metal contaminated soil passivator - Google Patents
The preparation method of organic-inorganic compoiste heavy-metal contaminated soil passivator Download PDFInfo
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- C09K17/40—Soil-conditioning materials or soil-stabilising materials containing mixtures of inorganic and organic compounds
Abstract
The invention discloses the preparation methods of organic-inorganic composite heavy-metal contaminated soil passivator, and this approach includes the following steps：1) bentonite is placed in baking oven, is dried 10 hours at 105 DEG C, it is spare；2) bentonite for weighing drying, it is 100mL to add water to be made into liquid-solid ratio：The suspension of 2 10g stirs 0.5 hour；3) sodium carbonate is added into above-mentioned suspension, is stirred to react at 70 DEG C 2 hours；4) modifying agent is added, is persistently stirred to react at 30 90 DEG C 1 10 hours；5) it after reaction, is cooled to room temperature, filters, it is 7.0 to be washed with deionized to pH value, 24 hours dry at 60 DEG C, and grinding sieves with 100 mesh sieve to get passivator finished product.Passivator of the present invention has the characteristics that raw material sources are extensive, cheap and natural free of contamination, and preparation method is simple, reaction condition is mild, and properties of product are stablized, there is passivation repairing effect well to heavy-metal contaminated soil, is applicable to the reparation of large area Compound Heavy Metals soil.
Description
Technical field
The present invention relates to a kind of preparation methods of heavy-metal contaminated soil passivator, belong to heavy metal-polluted soil in environmental protection
Pollution control field, specifically a kind of preparation method of organic-inorganic compoiste heavy-metal contaminated soil passivator.
Background technology
But with the development of industrial or agricultural, soil contamination problem getting worse seriously affects the development of national economy.Data sheet
It is bright, about 25,000,000 m of farm land area of China's heavy metal pollution2, annual contaminated by heavy metals grain up to 12,000,000 t,
Cause grain drop in production to be up to more than 1,000 ten thousand t because of heavy metal pollution, adds up at least 20,000,000,000 yuan of economic loss.Meanwhile huge sum of money accessory
There is non-biodegradable, larger harm not only generated to the yield and quality of crops, and be constantly enriched with by the transmission of food chain,
It is finally accumulated in human body and endangers health.Therefore, it is extremely urgent to reinforce heavy metal-polluted soil reparation.Soil restoring technology can be divided into
Physical technique, chemical technology and biotechnology：Peripheral doses technology includes barrier landfill, thermal desorption, electro reclamation etc., and chemistry is repaiied
Recovering technology includes passivation, elution technique etc., and biotechnology includes microorganism remediation, phytoremediation and animal reparation technology etc..Its
In, passivating technique has that easy to operate, the period is short, the advantages such as at low cost, applied widely, is large area heavy-metal contaminated soil
Reparation more preferably select, can meet the actual demand of current China's heavy-metal contaminated soil reparation well.
Passivating technique refers to being changed into heavy metal on physics and chemical property more by applying passivator into soil
Stable substance reduces the dissolubility of heavy metal, reduces to the influence caused by environment.Thus, the key of passivating technique application
It is passivator.Currently, Compound Heavy Metals soil is more and more, single passivator is difficult to reach the mark for repairing application
Standard plays the respective feature of passivator not of the same race then a variety of different type passivator can be used in combination, and enhancing passivation is repaiied
Reactivation power achievees the purpose that the soil of repairing heavy metal pollution.Accordingly, it is considered to by organic composite modified with inorganic passivant progress
Passivator is prepared, one side organic matter can buffer possible pH variations caused by chemical inactivators, on the other hand, organic matter
It can be combined to form compound with these inorganic passivants, play the role of preventing organic matter from degrading rapidly to a certain extent, because
And can overcome the disadvantages that because of risk caused by organic matter decomposition, achieve the effect that collaboration and complementation.
Bentonite is the nonmetallic ore using montmorillonite as essential mineral.Smectite structure is to press from both sides one by two oxygen-octahedrons
The 2 of layer alumina octahedral composition:1 type layer structure has stronger cation exchange capacity (CEC) because of its negatively charged.Due to mine
Adsorption effect, the exchange interaction of interlayer cation, the filtration in duct and the special two-dimensional nanostructure effect of object
Deng so that bentonite becomes passivator rare in heavy-metal contaminated soil reparation application.The layer structure of montmorillonite and
Strong ion-exchange capacity makes organic matter that may be adsorbed between montmorillonite lamella, becomes the bentonite modified organic and inorganic for preparing and answers
Fit theoretical foundation.Lot of documents shows：At normal temperatures and pressures, ion, water and salt and nearly all organic matter, can
The interlayer for enough passing in and out montmorillonite mineral, forms complicated montmorillonite inorganic complex or organic complex.It therefore, can be by that will have
Machine object monomer molecule or polymer long-chain are inserted into the piece interlayer of montmorillonite stratiform or are connected to montmorillonite surface, have prepared
Machine-inorganic composite type passivating material.Not only introduce the group strong to heavy metal adsorption, also increase the intergranular of montmorillonite away from,
So that montmorillonite is formd the porous active substance with microporous network structure, large specific surface area, further enhances bentonitic suction
Attached and ion-exchange performance achievees the purpose that improve bentonite passivation effect.
Invention content
Technical problem to be solved by the invention is to provide a kind of systems of organic-inorganic compoiste heavy metal soil passivator
Preparation Method, it is to prepare heavy-metal contaminated soil passivator by raw material of composite modified bentonite, and this method is with raw material
Source is extensive, cheap, good passivation effect, will not cause the advantages that secondary pollution.
In order to solve the above technical problems, the present invention uses following technical scheme：
The preparation method of organic-inorganic compoiste heavy metal soil passivator of the present invention, including following operating procedure：
The bentonite sieved with 100 mesh sieve is placed in baking oven by the first step, is dried 10 hours at 105 DEG C, is sealed and is protected after drying
It deposits, it is spare,
Second step weighs a certain amount of bentonite dried, and it is 100Ml to add water to be made into liquid-solid ratio：The suspension of 2-10g,
Stirring 0.5 hour,
Third walks, and sodium carbonate is added into above-mentioned suspension, is stirred to react at 70 DEG C 2 hours,
Suitable modifying agent is added in 4th step, is persistently stirred to react at 30-90 DEG C 1-10 hours,
5th step is cooled to room temperature after reaction, is filtered, and it is 7.0 to be washed with deionized to pH value, at 60 DEG C
24 hours dry, grinding sieves with 100 mesh sieve to get organic-inorganic compoiste heavy-metal contaminated soil passivator finished product.
In third step, the sodium carbonate of addition and the bentonite of drying are 0.05 in mass ratio：1.
In 4th step, the modifying agent of addition and the bentonite of drying are 1-20 in mass ratio：100.
In 4th step, the modifying agent is one or more kinds of in lignin, aminated lignin or sodium humate
Mixing.
The lignin and aminated lignin are respectively derived from the finished product and its amine of pulping and paper-making waste liquid acid adding precipitation filtering
Change product.
The preparation method of organic-inorganic compoiste heavy metal soil passivator of the present invention, compared with prior art, have with
Lower advantage：
(1) passivator of the present invention is made of natural substance modified, is not destroyed soil texture, is not generated secondary pollution, and
And it is cheap；
(2) lignin and sodium humate are connected to montmorillonite surface by the present invention by intercalation or ion-exchange reactions
And it is inserted into the piece interlayer of stratiform, the strong group of heavy metal adsorption is introduced, while increasing the interlamellar spacing of montmorillonite, keeps illiteracy de-
Stone forms the porous active substance with microporous network structure, large specific surface area, further enhance it is bentonitic absorption and from
Sub- switching performance forms organic-inorganic compoiste passivator, is applied in soil, can significantly improve bentonite to heavy metal soil
The passivation repairing effect of earth especially has good passivation repairing effect to Compound Heavy Metals soil；
(3) the heavy-metal contaminated soil passivator prepared by the method for the present invention is neutrality, has no toxic side effect to soil, is ring
Border friendly passivator；
(4) the method for the present invention preparation process is simple, and reaction condition is mild, and properties of product are stablized, and operability is strong.
Specific implementation mode
The method of the present invention is further described with reference to embodiment：
Embodiment 1, preparation method are：
(1) bentonite sieved with 100 mesh sieve is placed in baking oven, dries 10 hours at 105 DEG C, is sealed after drying, it is standby
With；
(2) bentonite for taking above-mentioned 10g to dry, it is 100mL to add water to be made into liquid-solid ratio：The suspension of 5g, stirring 0.5 are small
When；
(3) 0.5g sodium carbonate is added into above-mentioned suspension, is stirred to react at 70 DEG C 2 hours；
(4) 0.5g lignin is added, is persistently stirred to react at 75 DEG C 3 hours；
(5) after reaction, 25 DEG C are cooled to room temperature, is filtered, it is 7.0 to be washed with deionized to pH value, at 60 DEG C
24 hours dry, grinding sieves with 100 mesh sieve to get product passivator of the present invention.
Embodiment 2, preparation method are：
(1) bentonite sieved with 100 mesh sieve is placed in baking oven, dries 10 hours at 105 DEG C, is sealed after drying, it is standby
With；
(2) bentonite for taking above-mentioned 10g to dry, it is 100mL to add water to be made into liquid-solid ratio：The suspension of 2g, stirring 0.5
Hour；
(3) 0.5g sodium carbonate is added into above-mentioned suspension, is stirred to react at 70 DEG C 2 hours；
(4) 0.25g aminated lignins and 0.25g sodium humates is added, is persistently stirred to react at 45 DEG C 1 hour；
(5) after reaction, 25 DEG C are cooled to room temperature, is filtered, it is 7.0 to be washed with deionized to pH value, at 60 DEG C
24 hours dry, grinding sieves with 100 mesh sieve to get product passivator of the present invention.
Embodiment 3, preparation method are：
(1) bentonite sieved with 100 mesh sieve is placed in baking oven, dries 10 hours at 105 DEG C, is sealed after drying, it is standby
With；
(2) bentonite for taking above-mentioned 10g to dry, it is 100mL to add water to be made into liquid-solid ratio：The suspension of 10g, stirring 0.5
Hour；
(3) 0.5g sodium carbonate is added into above-mentioned suspension, is stirred to react at 70 DEG C 2 hours；
(4) 2g aminated lignins are added, are persistently stirred to react at 90 DEG C 7 hours；
(5) after reaction, 25 DEG C are cooled to room temperature, is filtered, it is 7.0 to be washed with deionized to pH value, at 60 DEG C
24 hours dry, grinding sieves with 100 mesh sieve to get product passivator of the present invention.
Embodiment 4, preparation method are：
(1) bentonite sieved with 100 mesh sieve is placed in baking oven, dries 10 hours at 105 DEG C, is sealed after drying,
It is spare；
(2) bentonite for taking above-mentioned 10g to dry, it is 100mL to add water to be made into liquid-solid ratio：The suspension of 8g, stirring 0.5 are small
When；
(3) 0.5g sodium carbonate is added into above-mentioned suspension, is stirred to react at 70 DEG C 2 hours；
(4) 0.1g aminated lignins are added, are persistently stirred to react at 90 DEG C 5 hours；
(5) after reaction, 25 DEG C are cooled to room temperature, is filtered, it is 7.0 to be washed with deionized to pH value, at 60 DEG C
24 hours dry, grinding sieves with 100 mesh sieve to get product passivator of the present invention.
Embodiment 5, preparation method are：
(1) bentonite sieved with 100 mesh sieve is placed in baking oven, dries 10 hours at 105 DEG C, is sealed after drying, it is standby
With；
(2) bentonite for taking above-mentioned 10g to dry, it is 100mL to add water to be made into liquid-solid ratio：The suspension of 5g, stirring 0.5
Hour；
(3) 0.5g sodium carbonate is added into above-mentioned suspension, is stirred to react at 70 DEG C 2 hours；
(4) 0.5g lignin and 0.5g sodium humates is added, is persistently stirred to react at 30 DEG C 10 hours；
(5) after reaction, 25 DEG C are cooled to room temperature, is filtered, it is 7.0 to be washed with deionized to pH value, at 60 DEG C
24 hours dry, grinding sieves with 100 mesh sieve to get product passivator of the present invention.
Embodiment 6, preparation method are：
(1) bentonite sieved with 100 mesh sieve is placed in baking oven, dries 10 hours at 105 DEG C, is sealed after drying, it is standby
With；
(2) bentonite for taking above-mentioned 10g to dry, it is 100mL to add water to be made into liquid-solid ratio：The suspension of 5g, stirring 0.5 are small
When；
(3) 0.5g sodium carbonate is added into above-mentioned suspension, is stirred to react at 70 DEG C 2 hours；
(4) 0.4g sodium humates are added, are persistently stirred to react at 75 DEG C 3 hours；
(5) after reaction, 25 DEG C are cooled to room temperature, is filtered, it is 7.0 to be washed with deionized to pH value, at 60 DEG C
24 hours dry, grinding sieves with 100 mesh sieve to get product passivator of the present invention.
Embodiment 7, preparation method are：
(1) bentonite sieved with 100 mesh sieve is placed in baking oven, dries 10 hours at 105 DEG C, is sealed after drying, it is standby
With；
(2) bentonite for taking above-mentioned 10g to dry, it is 100mL to add water to be made into liquid-solid ratio：The suspension of 8g, stirring 0.5 are small
When；
(3) 0.5g sodium carbonate is added into above-mentioned suspension, is stirred to react at 70 DEG C 2 hours；
(4) 0.25g lignin and 0.5g sodium humates is added, is persistently stirred to react at 60 DEG C 5 hours；
(5) after reaction, 25 DEG C are cooled to room temperature, is filtered, it is 7.0 to be washed with deionized to pH value, at 60 DEG C
24 hours dry, grinding sieves with 100 mesh sieve to get product passivator of the present invention.
Embodiment 8, preparation method are：
(1) bentonite sieved with 100 mesh sieve is placed in baking oven, dries 10 hours at 105 DEG C, is sealed after drying, it is standby
With；
(2) bentonite for taking above-mentioned 10g to dry, it is 100mL to add water to be made into liquid-solid ratio：The suspension of 5g, stirring 0.5
Hour；
(3) 0.5g sodium carbonate is added into above-mentioned suspension, is stirred to react at 70 DEG C 2 hours；
(4) 0.06g aminated lignins and 0.04g sodium humates is added, is persistently stirred to react at 45 DEG C 4 hours；
(5) after reaction, it is cooled to room temperature, filters, it is 7.0 to be washed with deionized to pH value, dry at 60 DEG C
24 hours, grinding sieved with 100 mesh sieve to get product passivator of the present invention.
Embodiment 9, preparation method are：
(1) bentonite sieved with 100 mesh sieve is placed in baking oven, dries 10 hours at 105 DEG C, is sealed after drying, it is standby
With；
(2) bentonite for taking above-mentioned 10g to dry, it is 100mL to add water to be made into liquid-solid ratio：The suspension of 10g, stirring 0.5
Hour；
(3) 0.5g sodium carbonate is added into above-mentioned suspension, is stirred to react at 70 DEG C 2 hours；
(4) 0.3g aminated lignins and 0.2g sodium humates is added, is persistently stirred to react at 60 DEG C 6 hours；
(5) after reaction, it is cooled to room temperature, filters, it is 7.0 to be washed with deionized to pH value, dry at 60 DEG C
24 hours, grinding sieved with 100 mesh sieve to get product passivator of the present invention.
Embodiment 10, preparation method are：
(1) bentonite sieved with 100 mesh sieve is placed in baking oven, dries 10 hours at 105 DEG C, is sealed after drying, it is standby
With；
(2) bentonite for taking above-mentioned 10g to dry, it is 100mL to add water to be made into liquid-solid ratio：The suspension of 2g, stirring 0.5 are small
When；
(3) 0.5g sodium carbonate is added into above-mentioned suspension, is stirred to react at 70 DEG C 2 hours；
(4) 0.6g aminated lignins and 0.4g sodium humates is added, is persistently stirred to react at 75 DEG C 2 hours；
(5) after reaction, it is cooled to room temperature, filters, it is 7.0 to be washed with deionized to pH value, dry at 60 DEG C
24 hours, grinding sieved with 100 mesh sieve to get product passivator of the present invention.
Test example 1
Heavy metal amount of capacity in simulation heavy metal wastewater thereby is adsorbed with modified product to be passivated to judge modified product heavy metal
Ability.Table 1 is suction of the organic-inorganic compoiste heavy metal soil passivator that is prepared of the method for the present invention to heavy metal ion
Attached ability.
Adsorption capacity of 1 passivator of the present invention of table to heavy metal ion
As shown in Table 1, the passivating agent products that the method for the present invention obtains can significantly improve bentonite to Cu2+、Pb2+、Zn2+、
Cd2+Adsorbance, be increased to respectively by original 25.65mg/g, 81.60mg/g, 26.55mg/g, 20.13mg/g maximum
53.18mg/g, 146.52mg/g, 66.98mg/g, 37.65mg/g, be respectively increased 107.3%, 79.6%, 152.3%,
87.0%.Meanwhile the present invention synthesizes passivator and prepares raw material --- bentonite, lignin and sodium humate be natural goods
Matter, and abundance, cheap and easy to get, therefore, the passivator being prepared is of low cost, to environment non-secondary pollution, while energy
Bentonitic added value is improved, there is good economy, environmental benefit.
Test example 2
Using laboratory simulation Compound Heavy Metals soil as experimental subjects, heavy metal concentration be cadmium 201.23mg/g,
Lead 1020.59mg/g, zinc 2024.68mg/g, copper 1021.76mg/g.Weigh the simulation weight of 50g natural air dryings, ground 1mm sieves
Metallic pollution pedotheque is placed in 250mL beakers, and the dosage of passivator of the present invention is soil quality 1%, 3%, 5%, is added
Entering a certain amount of distilled water makes soil moisture content be maintained at 30% or so, stirs evenly, and conserves 15 days respectively.After 15 days, takes and repair
Soil after multiple, the effect of passivator is determined using the leaching method of soil pH value and HJ/300-2007, and with unmodified swollen
Profit soil carries out contrast experiment.The results are shown in Table 2.
Passivation repair ability of 2 passivator of the present invention of table to Compound Heavy Metals soil
As shown in Table 2, the organic-inorganic compoiste heavy-metal contaminated soil passivator pair being prepared by the method for the present invention
Compound Heavy Metals soil has splendid passivation repairing effect, can effectively improve soil pH value, and it is passivated repair ability and shows
It writes and is better than unmodified bentonite.With the increase of passivator dosage, front and back Cu is repaired in simulation soil passivation2+、Pb2+、Zn2+、
Cd2+Leaching concentration continuously decreases, and soil pH value then gradually rises；Under the conditions of same passivator dosage, organic-inorganic compoiste
The Cu of soil after passivator is repaired2+、Pb2+、Zn2+、Cd2+Leaching concentration is below unmodified bentonite.Wherein it is passivated in the present invention
When the dosage of agent is 5%, the Cu of soil after reparation2+、Pb2+、Zn2+、Cd2+Leaching concentration be reduced to 0mg/L, 0.16mg/L,
2.69mg/L, 1.88mg/L reduce ratio respectively up to 100%, 99.82%, 98.28%, 83.81%.
Claims (4)
1. the preparation method of organic-inorganic compoiste heavy-metal contaminated soil passivator, which is characterized in that this method includes following
Operating procedure：
The bentonite sieved with 100 mesh sieve is placed in baking oven by the first step, is dried 10 hours at 105 DEG C, is sealed after drying, standby
With,
Second step weighs a certain amount of bentonite dried, and water is added to be made into the suspension that liquid-solid ratio is 100mL ︰ 2-10g, stirring
0.5 hour,
Third walks, and sodium carbonate is added into above-mentioned suspension, is stirred to react at 70 DEG C 2 hours,
Suitable modifying agent is added in 4th step, is persistently stirred to react at 30-90 DEG C 1-10 hours；The modifying agent is wooden
One or more kinds of mixing in element, aminated lignin or sodium humate；
5th step is cooled to room temperature after reaction, is filtered, and it is 7.0 to be washed with deionized to pH value, dry at 60 DEG C
24 hours, grinding sieved with 100 mesh sieve to get to organic-inorganic compoiste heavy-metal contaminated soil passivator finished product.
2. the preparation method of organic-inorganic compoiste heavy-metal contaminated soil passivator, feature exist according to claim 1
In：In third step, the sodium carbonate of addition and the bentonite of drying are 0.05 ︰ 1 in mass ratio.
3. the preparation method of organic-inorganic compoiste heavy-metal contaminated soil passivator, feature exist according to claim 1
In：In 4th step, the modifying agent of addition and the bentonite of drying are 1-20 ︰ 100 in mass ratio.
4. the preparation method of organic-inorganic compoiste heavy-metal contaminated soil passivator, feature exist according to claim 1
In：The lignin and aminated lignin are respectively derived from finished product and its amination production of pulping and paper-making waste liquid acid adding precipitation filtering
Product.
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| CN110467922A (en) * | 2019-07-12 | 2019-11-19 | 广东工业大学 | A kind of soil passivation modifying agent and its preparation method and application containing industrial lignin |
| CN111992258B (en) * | 2020-09-04 | 2023-03-21 | 广西大学 | Method for treating heavy metal pollution in sulfide ore tailings |
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