CN109762572A - A kind of preparation method of the reparation medicament of mercury contaminated soil - Google Patents
A kind of preparation method of the reparation medicament of mercury contaminated soil Download PDFInfo
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Abstract
The present invention relates to environment protection fields, particularly with regard to a kind of preparation method of the reparation medicament of mercury contaminated soil；A kind of preparation method of the reparation medicament of mercury contaminated soil disclosed in the method for the present invention, this patent is prepared for a kind of reparation medicament of mesoporous ceramic material as mercury contaminated soil, material specific surface area with higher and sulfur-bearing functional group abundant, it is capable of the mercury ion of each valence state in the absorption soil of effective selectivity, to reach the migration and biological effectiveness for reducing mercury element；This product is suitable for adsorbing passivating material as mercury metal, has that adsorption effect is prominent, production cost is low, does not have the advantages that secondary pollution.
Description
Technical field
The present invention relates to environment protection fields, particularly with regard to a kind of preparation method of the reparation medicament of mercury contaminated soil.
Background technique
Mercury vapour and mercury salt (in addition to some solubility are minimum such as mercuric sulphide) are all hypertoxic, oral, sucking or contact
After can lead to brain and hepatic injury.And mercury can accumulate in vivo, it is easy to by skin and respiratory tract and alimentary canal
It absorbs.So the soil of mercury pollution must be administered effectively, the physical and mental health of people not so can be endangered.
CN107384427A discloses a kind of for mercury contaminated soil high-efficiency compound stabilizer and mercury contaminated soil reparation
Method, compound stabilizer are made of oxidant, compound stabilizer and pH adjusting agent；The method of mercury contaminated soil reparation: by mercury dirt
Dye soil is crushed, sieving is handled, and takes the lower mercury contaminated soil particulate of sieve；In mercury contaminated soil particulate plus water moisturizing, then plus
Enter oxidizing agent solution, stir and heats carry out oxidation reaction；It adds vulcanization salting liquid and carries out vulcanization reaction；Add ferrous salt
Excess S2- is precipitated, clay mineral is added and humus is adsorbed, pH adjusting agent is added and adjusts mercury contaminated soil pH to 6
~7, maintenance 3 days or more；This method can carry out to variform mercury in mercury contaminated soil while stabilize solidification, and stabilize effect
Fruit is good and the period is short, and medicament stock source is wide, at low cost, is conducive to be widely applied.
CN102373161A relates to the use of environmental microorganism and carries out field of environmental improvement, specifically a kind of reduction seawater
The bacterium of middle mercury pollution and its application.The bacterium for reducing mercury pollution in seawater is Pseudomonasputida SP1, is preserved in
State's Microbiological Culture Collection administration committee common micro-organisms center (CGMCC)；The deposit date is on 06 01st, 2010；Number
For CGMCC No.3887.The bacterium Pseudomonas putida SP1 of mercury pollution can remove seawater ring in the reduction seawater
Mercury in border.The invention is using mercury pollution in bacterial strain SP1 removing seawater with high-efficient, nutritional requirement is low, easy to operate and peace
The advantages that Quan Xinggao, significantly reduces seawater mercury pollution and controls compared with other existing techniques
CN108339849A discloses a kind of soil-repairing agent and the method for renovation of organic pollution or mercury contaminated soil, the soil
Earth renovation agent includes pH 4-5, the solution of ferrous chloride that mass concentration is 3-5%, this is used for renovation of organic pollution or mercury pollution soil
The method of earth is the following steps are included: take organic contamination or mercury contaminated soil to be repaired；Prepare soil-repairing agent；By the soil
Renovation agent is added in the organic contamination to be repaired or mercury contaminated soil, is mixed and stirred for, obtains mixture；By the mixing
Material, which is placed in microwave reactor, to react, the soil after being repaired.The invention is intended to provide a kind of efficient rehabilitating soil, desorption rate
The soil-repairing agent and restorative procedure of high renovation of organic pollution or mercury contaminated soil.
Remediation of heavy metal-contaminated soil mainly have soil moved in improve the original soil replacement method, heat treating process, curing/stabilizing method, elution method,
Electro reclamation, biological restoration etc..The static stabilization of mercury in mercury contaminated soil may be implemented in these methods to a certain extent,
But because the mercury in soil often has a variety of valence states, the removal effect and stabilization effect of these methods are difficult to ensure.
Summary of the invention
To solve the above-mentioned problems, the present invention provides a kind of preparation methods of the reparation medicament of mercury contaminated soil.
A kind of preparation method of the reparation medicament of mercury contaminated soil, its technical solution is as follows:
According to mass fraction, 15-30 parts of sulfonated modified mesoporous ceramic carrier material is added to 150-180 parts of 0.1%-
It in the aqueous solution of 0.5% ammonium hydrogen phosphate, is dispersed with stirring uniformly, 40-60 DEG C of temperature control, 1-5 parts of calcium superphosphate is added, stirring is equal
1.6-4.2 parts of thiopropionamide is added in reaction kettle after even, 60-80 DEG C of temperature control, is stirred to react 1-5h；After completing reaction
Room temperature is cooled to, by 0.5-1.8 parts of 3- sulfydryl -1- propylamine, 0.01-0.5 parts of tetrachloro nickel acid tetraethyl ammoniums are added to reaction kettle
In, 60-180min is stirred at room temperature, is then allowed to stand 15-30h, completes to filter product after standing, be washed with deionized three times
The heated-air drying 1-5h for using 40-60 DEG C afterwards, then grinds, a kind of reparation medicament of mercury contaminated soil can be obtained.
The sulfonated modified mesoporous ceramic carrier material is prepared according to following scheme:
According to mass fraction, by 0.01-0.15 parts of surfactant diglycollic amide glycerol stearate monoesters and 0.5-1.8 parts
N- (6- Aminohexyl) amino methyl triethoxysilane 70%-90% for being added to 120-180 parts ethyl alcohol in, then will
10-20 parts of mesoporous ceramic carrier material is added in reaction kettle, ultrasonic disperse 20-30min, and 8-15 parts of concentrated hydrochloric acids are added,
0.01-0.5 parts of 3- indoleacetaldehydes are sour, after mixing evenly 50-70 DEG C of temperature control；Then 1-5 parts of 3- (trihydroxy silicon substrate) third is added
Alkyl sulfonic acid, 3 parts of bisindole maleimides of 0.01-0., is stirring evenly and then adding into 6.4-12.6 parts of hydrogen peroxide, continues to stir
30-60min is reacted, is first washed with acidic ethanol after filtering, is then washed with deionized, the sulphur can be obtained after dry
Acidified modified mesoporous ceramic carrier material.
The mesoporous ceramic carrier material average grain diameter is 5-50nm, and specific surface area is 500-1500 m2/g。
The reparation medicament of the mercury contaminated soil is when in use according to the ratio with contaminated soil mass ratio 4-15:1000
Application.
The reparation medicament of the mercury contaminated soil needs to guarantee that before use, soil pH value is 5-8.
A kind of preparation method of the reparation medicament of mercury contaminated soil, this patent disclosed in the method for the present invention are prepared in one kind
Reparation medicament of the hole ceramic material as mercury contaminated soil, material specific surface area with higher and sulfur-bearing function abundant
Group, is capable of the mercury ion of each valence state in the absorption soil of effective selectivity, to reach the migration and life for reducing mercury element
Object validity；This product is suitable for adsorbing passivating material as mercury metal, has that adsorption effect is prominent, production cost is low, without two
The advantages that secondary pollution.
Specific embodiment
The invention is described further below by specific embodiment:
Embodiment 1
A kind of preparation method of the reparation medicament of mercury contaminated soil, its technical solution is as follows:
According to mass fraction, 24 parts of sulfonated modified mesoporous ceramic carrier material is added to 170 parts of 0.3% phosphoric acid hydrogen
In the aqueous solution of ammonium, it is dispersed with stirring uniformly, 50 DEG C of temperature control, 3 parts of calcium superphosphate is added, it is thio by 3.4 parts after mixing evenly
Propionamide is added in reaction kettle, 70 DEG C of temperature control, is stirred to react 3h；Room temperature is cooled to after completing reaction, by 1.2 parts of 3- mercapto
Base -1- propylamine, 0.05 part of tetrachloro nickel acid tetraethyl ammonium is added in reaction kettle, 120min is stirred at room temperature, is then allowed to stand for 24 hours, complete
Product is filtered at after standing, is washed with deionized three times afterwards with 50 DEG C of heated-air drying 3h, is then ground, can be obtained one
The reparation medicament of kind mercury contaminated soil.
The sulfonated modified mesoporous ceramic carrier material is prepared according to following scheme:
According to mass fraction, by 0.1 part of surfactant diglycollic amide glycerol stearate monoesters and 0.9 part of N- (6- ammonia
Base hexyl) amino methyl triethoxysilane is added in 160 parts of 80% ethyl alcohol, then by 15 parts of mesoporous ceramic carrier
Material is added in reaction kettle, ultrasonic disperse 25min, 9 parts of concentrated hydrochloric acids is added, 0.03 part of 3- indoleacetaldehyde is sour, after mixing evenly
58 DEG C of temperature control；Then 3 parts 3- (trihydroxy silicon substrate) propane sulfonic acid is added, 0.07 part of bisindole maleimide stirs evenly
8 parts of hydrogen peroxide is added afterwards, continues to be stirred to react 50min, is first washed with acidic ethanol after filtering, be then washed with deionized water
It washs, the sulfonated modified mesoporous ceramic carrier material can be obtained after dry.
The mesoporous ceramic carrier material average grain diameter is 30nm, and specific surface area is 1000 m2/g。
The reparation medicament of the mercury contaminated soil of this experiment preparation, which is added to zeroth order mercury content according to the ratio of 12:1000, is
200mg/kg, Hg chloride content 3000mg/kg, pH value be 6 soil in, carry out repair process 30 days, nonvalent mercury migration
98.7% is reduced, mercury chloride migration reduces by 97.2%.
Embodiment 2
A kind of preparation method of the reparation medicament of mercury contaminated soil, its technical solution is as follows:
According to mass fraction, 15 parts of sulfonated modified mesoporous ceramic carrier material is added to 150 parts of 0.1% phosphoric acid hydrogen
In the aqueous solution of ammonium, it is dispersed with stirring uniformly, 40 DEG C of temperature control, 1 part of calcium superphosphate is added, it is thio by 1.6 parts after mixing evenly
Propionamide is added in reaction kettle, 60 DEG C of temperature control, is stirred to react 1h；Room temperature is cooled to after completing reaction, by 0.5 part of 3- mercapto
Base -1- propylamine, 0.01 part of tetrachloro nickel acid tetraethyl ammonium is added in reaction kettle, 60min is stirred at room temperature, is then allowed to stand 15h, complete
Product is filtered at after standing, is washed with deionized three times afterwards with 40 DEG C of heated-air drying 1h, is then ground, can be obtained one
The reparation medicament of kind mercury contaminated soil.
The sulfonated modified mesoporous ceramic carrier material is prepared according to following scheme:
According to mass fraction, by 0.01 part of surfactant diglycollic amide glycerol stearate monoesters and 0.5 part of N- (6- ammonia
Base hexyl) amino methyl triethoxysilane is added in 120 parts of 70% ethyl alcohol, then by 10 parts of mesoporous ceramic carrier
Material is added in reaction kettle, ultrasonic disperse 20min, 8 parts of concentrated hydrochloric acids is added, 0.01 part of 3- indoleacetaldehyde is sour, after mixing evenly
50 DEG C of temperature control；Then 1 part 3- (trihydroxy silicon substrate) propane sulfonic acid is added, 0.01 part of bisindole maleimide stirs evenly
6.4 parts of hydrogen peroxide is added afterwards, continues to be stirred to react 30min, is first washed with acidic ethanol after filtering, be then washed with deionized water
It washs, the sulfonated modified mesoporous ceramic carrier material can be obtained after dry.
The mesoporous ceramic carrier material average grain diameter is 50nm, and specific surface area is 500 m2/g。
The reparation medicament of the mercury contaminated soil of this experiment preparation, which is added to zeroth order mercury content according to the ratio of 4:1000, is
200mg/kg, Hg chloride content 3000mg/kg, pH value be 5 soil in, carry out repair process 30 days, nonvalent mercury migration
96.2% is reduced, mercury chloride migration reduces by 94.8%.
Embodiment 3
A kind of preparation method of the reparation medicament of mercury contaminated soil, its technical solution is as follows:
According to mass fraction, 30 parts of sulfonated modified mesoporous ceramic carrier material is added to 180 parts of 0.5% phosphoric acid hydrogen
In the aqueous solution of ammonium, it is dispersed with stirring uniformly, 60 DEG C of temperature control, 5 parts of calcium superphosphate is added, it is thio by 4.2 parts after mixing evenly
Propionamide is added in reaction kettle, 80 DEG C of temperature control, is stirred to react 5h；Room temperature is cooled to after completing reaction, by 1.8 parts of 3- mercapto
Base -1- propylamine, 0.5 part of tetrachloro nickel acid tetraethyl ammonium is added in reaction kettle, 180min is stirred at room temperature, is then allowed to stand 30h, complete
Product is filtered at after standing, is washed with deionized three times afterwards with 60 DEG C of heated-air drying 5h, is then ground, can be obtained one
The reparation medicament of kind mercury contaminated soil.
The sulfonated modified mesoporous ceramic carrier material is prepared according to following scheme:
According to mass fraction, by 0.15 part of surfactant diglycollic amide glycerol stearate monoesters and 1.8 parts of N- (6- ammonia
Base hexyl) the amino methyl triethoxysilane 70%-90% that is added to 180 parts ethyl alcohol in, then by 20 parts of mesoporous ceramic
Carrier material is added in reaction kettle, ultrasonic disperse 30min, 15 parts of concentrated hydrochloric acids is added, 0.5 part of 3- indoleacetaldehyde acid, stirring is
70 DEG C of temperature control after even；Then 5 parts 3- (trihydroxy silicon substrate) propane sulfonic acid, 0. 3 parts of bisindole maleimides, stirring is added
12.6 parts of hydrogen peroxide is added after uniformly, continues to be stirred to react 60min, first be washed with acidic ethanol after filtering, then spend from
The sulfonated modified mesoporous ceramic carrier material can be obtained after dry in sub- water washing.
The mesoporous ceramic carrier material average grain diameter is 5nm, and specific surface area is 1500 m2/g。
The reparation medicament of the mercury contaminated soil of this experiment preparation, which is added to zeroth order mercury content according to the ratio of 15:1000, is
200mg/kg, Hg chloride content 3000mg/kg, pH value be 8 soil in, carry out repair process 30 days, nonvalent mercury migration
99.7% is reduced, mercury chloride migration reduces by 98.4%.
Embodiment 4
A kind of preparation method of the reparation medicament of mercury contaminated soil, its technical solution is as follows:
According to mass fraction, 30 parts of sulfonated modified mesoporous ceramic carrier material is added to 180 parts of 0.5% phosphoric acid hydrogen
In the aqueous solution of ammonium, it is dispersed with stirring uniformly, 60 DEG C of temperature control, 5 parts of calcium superphosphate is added, it is thio by 4.2 parts after mixing evenly
Propionamide is added in reaction kettle, 80 DEG C of temperature control, is stirred to react 5h；Room temperature is cooled to after completing reaction, by 1.8 parts of 3- mercapto
Base -1- propylamine, 0.05 part of tetrachloro nickel acid tetraethyl ammonium are added in reaction kettle, 180min are stirred at room temperature, is then allowed to stand 30h,
It completes to filter product after standing, is washed with deionized three times afterwards with 60 DEG C of heated-air drying 5h, then grinds, can be obtained
A kind of reparation medicament of mercury contaminated soil.
The sulfonated modified mesoporous ceramic carrier material is prepared according to following scheme:
According to mass fraction, by 0.05 part of surfactant diglycollic amide glycerol stearate monoesters and 0.5 part of N- (6- ammonia
Base hexyl) amino methyl triethoxysilane is added in 180 parts of 90% ethyl alcohol, then by 15 parts of mesoporous ceramic carrier
Material is added in reaction kettle, ultrasonic disperse 20min, 15 parts of concentrated hydrochloric acids is added, 0.01 part of 3- indoleacetaldehyde is sour, after mixing evenly
70 DEG C of temperature control；Then 1 part 3- (trihydroxy silicon substrate) propane sulfonic acid is added, 0. 3 parts of bisindole maleimides, stirring is
6.4 parts of hydrogen peroxide is added after even, continues to be stirred to react 60min, is first washed with acidic ethanol after filtering, then use deionized water
The sulfonated modified mesoporous ceramic carrier material can be obtained after dry in washing.
The mesoporous ceramic carrier material average grain diameter is 10nm, and specific surface area is 1272 m2/g。
The reparation medicament of the mercury contaminated soil of this experiment preparation, which is added to zeroth order mercury content according to the ratio of 5:1000, is
200mg/kg, Hg chloride content 3000mg/kg, pH value be 7 soil in, carry out repair process 30 days, nonvalent mercury migration
96.7% is reduced, mercury chloride migration reduces by 95.3%.
Comparative example 1
Tetrachloro nickel acid tetraethyl ammonium, the other the same as in Example 1 was not added.
This experiment nonvalent mercury migration is reduced by 93.1%, mercury chloride migration reduces by 89.4%.
Comparative example 2
3- indoleacetaldehyde acid, the other the same as in Example 1 is not added.
This experiment nonvalent mercury migration is reduced by 88.2%, mercury chloride migration reduces by 89.5%.
Comparative example 3
3- sulfydryl -1- propylamine, the other the same as in Example 1 is not added.
This experiment nonvalent mercury migration is reduced by 78.5%, mercury chloride migration reduces by 74.8%.
Comparative example 4
3- (trihydroxy silicon substrate) propane sulfonic acid, the other the same as in Example 1 is not added.
This experiment nonvalent mercury migration is reduced by 73.1%, mercury chloride migration reduces by 69.7%.
Comparative example 5
N- (6- Aminohexyl) amino methyl triethoxysilane, the other the same as in Example 1 is not added.
This experiment nonvalent mercury migration is reduced by 67.8%, mercury chloride migration reduces by 66.1%.
Comparative example 6
Bisindole maleimide, the other the same as in Example 1 is not added.
This experiment nonvalent mercury migration is reduced by 89.8%, mercury chloride migration reduces by 86.1%.
Claims (5)
1. a kind of preparation method of the reparation medicament of mercury contaminated soil, its technical solution is as follows:
According to mass fraction, 15-30 parts of sulfonated modified mesoporous ceramic carrier material is added to 150-180 parts of 0.1%-
It in the aqueous solution of 0.5% ammonium hydrogen phosphate, is dispersed with stirring uniformly, 40-60 DEG C of temperature control, 1-5 parts of calcium superphosphate is added, stirring is equal
1.6-4.2 parts of thiopropionamide is added in reaction kettle after even, 60-80 DEG C of temperature control, is stirred to react 1-5h；After completing reaction
Room temperature is cooled to, by 0.5-1.8 parts of 3- sulfydryl -1- propylamine, 0.01-0.5 parts of tetrachloro nickel acid tetraethyl ammoniums are added to reaction kettle
In, 60-180min is stirred at room temperature, is then allowed to stand 15-30h, completes to filter product after standing, be washed with deionized three times
The heated-air drying 1-5h for using 40-60 DEG C afterwards, then grinds, a kind of reparation medicament of mercury contaminated soil can be obtained.
2. a kind of preparation method of the reparation medicament of mercury contaminated soil according to claim 1, it is characterised in that: described
Sulfonated modified mesoporous ceramic carrier material is prepared according to following scheme:
According to mass fraction, by 0.01-0.15 parts of surfactant diglycollic amide glycerol stearate monoesters and 0.5-1.8 parts
N- (6- Aminohexyl) amino methyl triethoxysilane 70%-90% for being added to 120-180 parts ethyl alcohol in, then will
10-20 parts of mesoporous ceramic carrier material is added in reaction kettle, ultrasonic disperse 20-30min, and 8-15 parts of concentrated hydrochloric acids are added,
0.01-0.5 parts of 3- indoleacetaldehydes are sour, after mixing evenly 50-70 DEG C of temperature control；Then 1-5 parts of 3- (trihydroxy silicon substrate) third is added
Alkyl sulfonic acid, 3 parts of bisindole maleimides of 0.01-0., is stirring evenly and then adding into 6.4-12.6 parts of hydrogen peroxide, continues to stir
30-60min is reacted, is first washed with acidic ethanol after filtering, is then washed with deionized, the sulphur can be obtained after dry
Acidified modified mesoporous ceramic carrier material.
3. a kind of preparation method of the reparation medicament of mercury contaminated soil according to claim 2, it is characterised in that: described
Mesoporous ceramic carrier material average grain diameter is 5-50nm, and specific surface area is 500-1500 m2/g。
4. a kind of preparation method of the reparation medicament of mercury contaminated soil according to claim 1, it is characterised in that: described
The reparation medicament of mercury contaminated soil is applied according to the ratio of contaminated soil mass ratio 4-15:1000 when in use.
5. a kind of preparation method of the reparation medicament of mercury contaminated soil according to claim 1, it is characterised in that: described
The reparation medicament of mercury contaminated soil needs to guarantee that before use, soil pH value is 5-8.
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| CN102389776A (en) * | 2011-10-09 | 2012-03-28 | 广东省生态环境与土壤研究所 | Metal heavy absorbent and preparation method and use thereof |
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