CN106582537A - Preparation method and product of composite material for repairing soil contaminated by heavy metal - Google Patents
Preparation method and product of composite material for repairing soil contaminated by heavy metal Download PDFInfo
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- CN106582537A CN106582537A CN201611147107.4A CN201611147107A CN106582537A CN 106582537 A CN106582537 A CN 106582537A CN 201611147107 A CN201611147107 A CN 201611147107A CN 106582537 A CN106582537 A CN 106582537A
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- 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
- B01J20/223—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material containing metals, e.g. organo-metallic compounds, coordination complexes
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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
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- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
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Abstract
The invention provides a preparation method of a composite material for repairing soil contaminated by heavy metal. The composite material capable of being used for efficiently repairing the farmland soil heavy metal Cd is successfully synthesized, a higher adsorption amount and a more durable passivation effect are achieved for the heavy metal Cd; materials which are used are low in price and easy to obtain, and large-area application and popularization of soil heavy metal passivation repair in contaminated regions in China are facilitated; main adsorption functional groups, namely, sulfydryl groups (-HS), amino groups and DTPA in an insertion layer can be efficiently complexed with heavy metal ions, a stable complex is generated, and an ideal effect can be achieved for the passivation repair of the heavy metal contaminating the soil; and the composite material is moderate in density and fine in particle, the composite material is uniform when mixed in soil, and applicability of the composite material is enhanced.
Description
Technical field
The invention belongs to field of environment engineering technology, more particularly, to a kind of composite of restoration of soil polluted by heavy metal
Preparation method and product.
Background technology
With developing rapidly for industrialization and urbanization, heavy metal pollution of soil is into the great attention for causing the mankind.
The most of arable land of China is extremely serious by heavy metal pollutions such as Cd, As, Pb, Hg, Zn.It not only to ecological environmental danger,
Biological growth and development are affected, but also human body can be entered by food chain, jeopardize existence and the health of the mankind.Cadmium rice,
The heavy metal pollutions such as arsenic poison, blood lead endanger all reports common in recent years, and " minamata disease " and " Itai-itai diseases " is ascertained respectively by a huge sum of money
Category Hg and Cd pollutions cause, and heavy metal pollution problem causes the common concern of countries in the world.
Have many kinds with regard to heavy metal-polluted soil Cd pollution amelioration methods, generally include physical restoration, chemical restoration and
Biological restoration.Passivation reparation in chemical restoration has the advantages that in situ, simple, easy to operate.But do not have all the time all the time
Have and find good heavy metal-polluted soil passivation reparation chemical material.
The content of the invention
In view of this, it is contemplated that propose a kind of composite of remediating heavy metal Cd contaminated soils preparation method and
Product, with provide it is a kind of with universal, be capable of the composite of efficient rehabilitating soil heavy metal pollution.
To reach above-mentioned purpose, the technical scheme is that what is be achieved in that：
A kind of preparation method of the composite of restoration of soil polluted by heavy metal, the synthesis step of DTPA intercalated houghites
For：
(1) will be MgCl26H2O and AlCl36H2O soluble in water, stirring obtains mixture；
(2) ammonia is added in mixture, a period of time is stood after being sufficiently stirred for；
(3) diethyl pentetic acid is added in the system after standing, stir, it is aging；
(4) the sample lyophilization for obtaining (3) step, obtains DTPA intercalated houghite nano-scale particles.
In step (1), water is deionized water, and MgCl26H2O is 1 with the weight ratio of deionized water:30-40, AlCl3
6H2O is 1 with the weight ratio of deionized water:15-20, stirs 5-10min under conditions of 500-1000 rev/min.
In step (2), ammonia and the weight ratio of deionized water in step (1) step are 1:20-40, at 200-700 rev/min
Under the conditions of stir 1-5min after, stand 10-20min.
In step (3), diethyl pentetic acid and the weight ratio of deionized water in step (1) step are 1:20-25,
15-20min, aging 60-80min are stirred under the conditions of 500-1000 rev/min.
The sample in step (4) obtaining (3) step lyophilization 20-25h under the conditions of (- 50 DEG C)-(- 60 DEG C) is obtained
DTPA intercalated houghite nano-scale particles.
By the DTPA intercalations described in sulfydryl modification meerschaum, amido modified attapulgite clay and any one of claim 1-5
Brucite mixes.
The weight ratio of sulfydryl modification meerschaum, amido modified attapulgite clay and DTPA intercalated houghites is (2-4)：(2-
3)：1.
The synthesis step of the sulfydryl modification meerschaum is:
(1) natural sepiolite is scattered in deionized water, natural sepiolite is 1 with the weight ratio of deionized water:5,
7min is stirred under conditions of 1000 revs/min, meerschaum suspension is formed；
(2) meerschaum suspension is placed on dispersion machine, 23min is stirred under conditions of 10000 revs/min, form Hai Pao
Stone colloid；
(3) mercaptopropyl trimethoxysilane, step are added in meerschaum colloid under 8000 revs/min of stirring condition
(1) in, natural sepiolite and the weight ratio of mercaptopropyl trimethoxysilane are 330:29, after stirring 5min, mixing speed is adjusted
For 10000 revs/min, continue stirring 12min, form meerschaum gelinite；
(4) by meerschaum gelinite, under the conditions of 70 DEG C, constant temperature stands 40h, and colloid Hai Pao is taken out from meerschaum gelinite
Stone, dries under the conditions of 65 DEG C, sulfydryl modification meerschaum is obtained after grinding.
The synthesis step of the amido modified attapulgite clay is：
(1) attapulgite clay is scattered in the aqueous solution of the cetyl trimethylammonium bromide that concentration is 2%, attapulgite
Clay compares 1 with the weight of cetyl trimethylammonium bromide:3, form attapulgite clay suspension；
(2) attapulgite clay suspension is stood after 24h, is placed on dispersion machine, stirred with 1700 revs/min of speed
12min, obtains attapulgite clay colloid；
(3) under conditions of 1000 revs/min, aminopropyl triethoxysilane, step are added in attapulgite clay gel
(1) in, attapulgite clay and the weight ratio of aminopropyl triethoxysilane are 330:21, continue the bar at 1500-2000 rev/min
15min is stirred under part, attapulgite clay gelinite is formed；
(4) natural air drying, the grinding under the conditions of 30 DEG C by attapulgite clay gelinite, obtains amido modified attapulgite
Clay particle.
Relative to prior art, a kind of composite of restoration of soil polluted by heavy metal of the present invention has following excellent
Gesture：
A kind of preparation method of the composite of restoration of soil polluted by heavy metal that the present invention is provided, successfully synthesizing can be with
For the composite for efficiently repairing farmland soil heavy metals Cd, heavy metal Cd has higher adsorbance, more longlasting passivation
Effect；And material therefor is cheap and easy to get, is conducive to heavy metal-polluted soil passivation to repair and pushes away in the contaminated regional large area of China
It is wide to apply；The DTPA of main adsorption functional group sulfydryl (- HS), amino and intercalation in composite can efficient complexing heavy metal
Ion, and stable complex is generated, the passivation reparation to Heavy Metals in Soil Contaminated can reach comparatively ideal effect；Composite wood
Material medium density, granule is thinner, is blended in more uniform in soil, enhances its suitability.
Specific embodiment
In addition to being defined, in following examples, technical term used is with universal with those skilled in the art of the invention
The identical meanings of understanding.In following examples, test reagent used, if no special instructions, is routine biochemistry reagent；It is described
Experimental technique, if no special instructions, is conventional method.
The present invention is described in detail with reference to embodiment.
Embodiment 1：
The synthesis step of DTPA intercalated houghites is：
(1) 75 parts of MgCl26H2O and 150 part of AlCl36H2O are dissolved in 3000 parts of water, in 500 revs/min of condition
Lower stirring 10min obtains mixture.
(2) 75 parts of ammonia are added in mixture, after 5min being stirred under conditions of 200 revs/min, stand 10min.
(3) 120 parts of diethyl pentetic acids are added in the system after standing, is stirred under the conditions of 500 revs/min
20min, aging 60min.
(4) sample for obtaining (3) step lyophilization 30h under the conditions of -60 DEG C, obtains DTPA intercalated houghite nanoscales
Granule.
Embodiment 2：
The synthesis step of DTPA intercalated houghites is：
(1) 80 parts of MgCl26H2O and 160 part of AlCl36H2O are dissolved in 3000 parts of water, in 650 revs/min of condition
Lower stirring 8.5min obtains mixture.
(2) 90 parts of ammonia are added in mixture, after 4min being stirred under conditions of 350 revs/min, stand 12.5min.
(3) 125 parts of diethyl pentetic acids are added in the system after standing, is stirred under the conditions of 650 revs/min
18.5min, aging 65min.
(4) sample for obtaining (3) step lyophilization 27h under the conditions of -57 DEG C, obtains DTPA intercalated houghite nanoscales
Granule.
Embodiment 3：
The synthesis step of DTPA intercalated houghites is：
(1) 85.7 parts of MgCl26H2O and 166.7 part of AlCl36H2O are dissolved in 3000 parts of water, at 800 revs/min
Under the conditions of stir 7min obtain mixture.
(2) 100 parts of ammonia are added in mixture, after 2.5min being stirred under conditions of 500 revs/min, stand 15min.
(3) 130 parts of diethyl pentetic acids are added in the system after standing, is stirred under the conditions of 800 revs/min
17min, aging 70min.
(4) sample for obtaining (3) step lyophilization 24h under the conditions of -55 DEG C, obtains DTPA intercalated houghite nanoscales
Granule.
Embodiment 4：
The synthesis step of DTPA intercalated houghites is：
(1) 90 parts of MgCl26H2O and 180 part of AlCl36H2O are dissolved in 3000 parts of water, in 900 revs/min of condition
Lower stirring 6min obtains mixture.
(2) 130 parts of ammonia are added in mixture, after 2min being stirred under conditions of 600 revs/min, stand 17.5min.
(3) 140 parts of diethyl pentetic acids are added in the system after standing, is stirred under the conditions of 900 revs/min
16.5min, aging 75min.
(4) sample for obtaining (3) step lyophilization 22h under the conditions of -53 DEG C, obtains DTPA intercalated houghite nanoscales
Granule.
Embodiment 5：
The synthesis step of DTPA intercalated houghites is：
(1) 100 parts of MgCl26H2O and 200 part of AlCl36H2O are dissolved in 3000 parts of water, in 1000 revs/min of bar
5min is stirred under part and obtains mixture.
(2) 150 parts of ammonia are added in mixture, after 1min being stirred under conditions of 700 revs/min, stand 20min.
(3) 150 parts of diethyl pentetic acids are added in the system after standing, is stirred under the conditions of 1000 revs/min
15min, aging 80min.
(4) sample for obtaining (3) step lyophilization 20h under the conditions of -50 DEG C, obtains DTPA intercalated houghite nanoscales
Granule.
Pedotheque, in greenhouse, is crossed 4mm sieves, respectively loaded on flowerpot by collection Chenzhou, Hunan Province rice field topsoil sample
In, soil 5 × 10 is filled in each flowerpot6G, in each flowerpot, the injected volume of metal Cd is 13g.
Respectively DTPA intercalated houghite 15.4g in Example 1-5, are separately added in 5 flowerpots, and the paddy growth cycle is
122.7 days, detect that the adsorption rate of heavy metal Cd is (the Cd contents in 13g- Oryza sativa L.)/13g, testing result is as shown in table 1：
Table 1
| DTPA intercalated houghites (15.4g) | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 |
| Adsorption rate (%) | 11.2 | 12.4 | 13.3 | 12.7 | 11.8 |
As a result show：Adsorption efficiency of the DTPA intercalated houghites obtained under the conditions of embodiment 3 to heavy metal in soil Cd
It is best.
Embodiment 6-12 is sulfydryl modification meerschaum, amido modified attapulgite clay, the three kinds of reparations of DTPA intercalated houghites
Material mixes in varing proportions；Comparative example 1-3 is sulfydryl modification meerschaum, amido modified attapulgite clay, DTPA intercalation neatlys
Any one material in three kinds of repair materials of stone；Comparative example 4-6 be sulfydryl modification meerschaum, amido modified attapulgite clay,
The mixing of any bi-material in three kinds of materials of DTPA intercalated houghites, as shown in table 2：DTPA intercalated houghites are in embodiment
Prepare under the conditions of 3；Sulfydryl modification meerschaum is as follows with the synthesis step of amido modified attapulgite clay：
The synthesis step of sulfydryl modification meerschaum is:
(1) 450 parts of natural sepiolites are scattered in 2250 parts of deionized waters, are stirred under conditions of 1000 revs/min
7min, forms meerschaum suspension；
(2) meerschaum suspension is placed on dispersion machine, 23min is stirred under conditions of 10000 revs/min, form Hai Pao
Stone colloid；
(3) under 8000 revs/min of stirring condition in meerschaum colloid add 39.5 parts of mercaptopropyl trimethoxysilanes,
After stirring 5min, mixing speed is adjusted to into 10000 revs/min, continues stirring 12min, form meerschaum gelinite；
(4) by meerschaum gelinite, under the conditions of 70 DEG C, constant temperature stands 40h, and colloid Hai Pao is taken out from meerschaum gelinite
Stone, dries under the conditions of 65 DEG C, sulfydryl modification meerschaum is obtained after grinding.
The synthesis step of amido modified attapulgite clay is：
(1) 450 parts of attapulgite clays are scattered in into the water-soluble of 1350 parts of cetyl trimethylammonium bromide that concentration is 2%
In liquid, attapulgite clay suspension is formed；
(2) attapulgite clay suspension is stood after 24h, is placed on dispersion machine, stirred with 1700 revs/min of speed
12min, obtains attapulgite clay colloid；
(3) under conditions of 1000 revs/min, 29.3 parts of aminopropyl-triethoxy silicon are added in attapulgite clay gel
Alkane, continuation stir 15min under conditions of 1500-2000 rev/min, form attapulgite clay gelinite；
(4) natural air drying, the grinding under the conditions of 30 DEG C by attapulgite clay gelinite, obtains amido modified attapulgite
Clay particle.
Pedotheque, in greenhouse, is crossed 4mm sieves, respectively loaded on flowerpot by collection Chenzhou, Hunan Province rice field topsoil sample
In, soil 5 × 10 is filled in each flowerpot6G, all material for preparing in Example 16-12 and in comparative example 1-6 respectively add respectively
Enter in a flowerpot, in each flowerpot, the injected volume of metal Cd is 13g, and mix homogeneously, paddy growth cycle are 122.7 days, inspection
The adsorption rate for surveying heavy metal Cd is (the Cd contents in 13g- Oryza sativa L.)/13g, and testing result is as shown in table 2：
Table 2
As a result show：When the gross mass of composite is identical, sulfydryl modification sepiolite particle, amido modified attapulgite clay
And the mixed proportion of DTPA intercalated houghites is 3:2.5:When 1, the repairing effect of composite is best；In sulfydryl modification meerschaum
The mixed proportion of granule, amido modified attapulgite clay and DTPA intercalated houghites is 3:2.5:When 1, the gross mass of composite
Bigger, repairing effect is better；When the gross mass of repair materials is identical, containing sulfydryl modification sepiolite particle, amido modified recessed
The repairing effect of the composite of three kinds of materials of convex rod clay and DTPA intercalated houghites is better than and comprises only in three kinds of repair materials
Any two kinds of repairing effect, the repairing effect for comprising only the composite of bi-material are better than and comprise only any of which material
The repairing effect of material.
Presently preferred embodiments of the present invention is the foregoing is only, not to limit the present invention, all essences in the present invention
Within god and principle, any modification, equivalent substitution and improvements made etc. should be included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of the composite of restoration of soil polluted by heavy metal, it is characterised in that：DTPA intercalated houghites
Synthesis step is：
(1) will be MgCl26H2O and AlCl36H2O soluble in water, stirring obtains mixture；
(2) ammonia is added in mixture, a period of time is stood after being sufficiently stirred for；
(3) diethyl pentetic acid is added in the system after standing, stir, it is aging；
(4) the sample lyophilization for obtaining (3) step, obtains DTPA intercalated houghite nano-scale particles.
2. the preparation method of the composite of a kind of restoration of soil polluted by heavy metal according to claim 1, its feature exist
In：In step (1), water is deionized water, and MgCl26H2O is 1 with the weight ratio of deionized water:30-40, AlCl36H2O with
The weight ratio of deionized water is 1:15-20, stirs 5-10min under conditions of 500-1000 rev/min.
3. the preparation method of the composite of a kind of restoration of soil polluted by heavy metal according to claim 1, its feature exist
In：In step (2), ammonia and the weight ratio of deionized water in step (1) step are 1:20-40, under conditions of 200-700 rev/min
After stirring 1-5min, 10-20min is stood.
4. the preparation method of the composite of a kind of restoration of soil polluted by heavy metal according to claim 1, its feature exist
In：In step (3), diethyl pentetic acid and the weight ratio of deionized water in step (1) step are 1:20-25, in 500-1000
15-20min, aging 60-80min are stirred under the conditions of rev/min.
5. the preparation method of the composite of a kind of restoration of soil polluted by heavy metal according to claim 1, its feature exist
In：The sample in step (4) obtaining (3) step lyophilization 20-25h under the conditions of (- 50 DEG C)-(- 60 DEG C) obtains DTPA and inserts
Layer hydrotalcite nano grade particles.
6. a kind of preparation method of the composite of restoration of soil polluted by heavy metal, it is characterised in that：By sulfydryl modification meerschaum,
DTPA intercalated houghites mixing described in amido modified attapulgite clay and any one of claim 1-5.
7. the preparation method of the composite of a kind of restoration of soil polluted by heavy metal according to claim 6, its feature exist
In：The weight ratio of sulfydryl modification meerschaum, amido modified attapulgite clay and DTPA intercalated houghites is (2-4)：(2-3)：1.
8. the preparation method of the composite of a kind of restoration of soil polluted by heavy metal according to claim 7, its feature exist
In：The synthesis step of the sulfydryl modification meerschaum is:
(1) natural sepiolite is scattered in deionized water, natural sepiolite is 1 with the weight ratio of deionized water:5,1000
7min is stirred under conditions of rev/min, meerschaum suspension is formed；
(2) meerschaum suspension is placed on dispersion machine, 23min is stirred under conditions of 10000 revs/min, form meerschaum glue
Body；
(3) mercaptopropyl trimethoxysilane is added in meerschaum colloid under 8000 revs/min of stirring condition, in step (1)
Natural sepiolite is 330 with the weight ratio of mercaptopropyl trimethoxysilane:29, after stirring 5min, mixing speed is adjusted to
10000 revs/min, continue stirring 12min, form meerschaum gelinite；
(4) by meerschaum gelinite, under the conditions of 70 DEG C, constant temperature stands 40h, and colloid meerschaum is taken out from meerschaum gelinite,
Dry under the conditions of 65 DEG C, after grinding, obtain sulfydryl modification meerschaum.
9. the preparation method of the composite of a kind of restoration of soil polluted by heavy metal according to claim 7, its feature exist
In：The synthesis step of the amido modified attapulgite clay is：
(1) attapulgite clay is scattered in the aqueous solution of the cetyl trimethylammonium bromide that concentration is 2%, attapulgite clay
Compare 1 with the weight of cetyl trimethylammonium bromide:3, form attapulgite clay suspension；
(2) attapulgite clay suspension is stood after 24h, is placed on dispersion machine, with 1700 revs/min of speed stirring 12min, obtained
To attapulgite clay colloid；
(3) under conditions of 1000 revs/min, aminopropyl triethoxysilane is added in attapulgite clay gel, in step (1)
Attapulgite clay is 330 with the weight ratio of aminopropyl triethoxysilane:21, continuation is stirred under conditions of 1500-2000 rev/min
15min is mixed, attapulgite clay gelinite is formed；
(4) natural air drying, the grinding under the conditions of 30 DEG C by attapulgite clay gelinite, obtains amido modified attapulgite clay
Granule.
10. a kind of composite of restoration of soil polluted by heavy metal, it is characterised in that：According to any one of claim 6-9 institute
A kind of preparation method of the composite of the restoration of soil polluted by heavy metal stated is prepared.
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| CN111575012A (en) * | 2020-05-22 | 2020-08-25 | 苏州市相润土壤修复技术研究院有限公司 | Composite material for passivating soil heavy metal nickel and preparation and application methods thereof |
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| CN108928880A (en) * | 2018-08-10 | 2018-12-04 | 南华大学 | A kind of processing method of the waste water containing radioactive element |
| CN108928880B (en) * | 2018-08-10 | 2021-07-09 | 南华大学 | Method for treating wastewater containing radioactive elements |
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| CN109621921B (en) * | 2019-01-30 | 2022-01-07 | 浙江省环境科技有限公司 | Sphere-like composite adsorbent for sewage treatment |
| CN110898797A (en) * | 2019-11-27 | 2020-03-24 | 清华大学深圳国际研究生院 | Preparation method of layered double hydroxide, layered double hydroxide and application |
| CN111575012A (en) * | 2020-05-22 | 2020-08-25 | 苏州市相润土壤修复技术研究院有限公司 | Composite material for passivating soil heavy metal nickel and preparation and application methods thereof |
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