CN106947486B - A kind of attapulgite-activated carbon from activated sludge soil remediation material and preparation method thereof - Google Patents
A kind of attapulgite-activated carbon from activated sludge soil remediation material and preparation method thereof Download PDFInfo
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- CN106947486B CN106947486B CN201710239445.9A CN201710239445A CN106947486B CN 106947486 B CN106947486 B CN 106947486B CN 201710239445 A CN201710239445 A CN 201710239445A CN 106947486 B CN106947486 B CN 106947486B
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- attapulgite
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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
- C09K17/02—Soil-conditioning materials or soil-stabilising materials containing inorganic compounds only
- C09K17/04—Soil-conditioning materials or soil-stabilising materials containing inorganic compounds only applied in a physical form other than a solution or a grout, e.g. as granules or gases
Abstract
The invention belongs to the higher value application field of biomass resource, in particular to a kind of attapulgite-activated carbon from activated sludge soil remediation material and preparation method thereof.Using attapulgite and the vegetable seed dregs of fat as raw material, attapulgite/carbon composite is prepared using a step high temperature pyrolytic cracking (HTP) first, then attapulgite/absorbent charcoal composite material as made from acid activation processing.
Description
Technical field
The invention belongs to the higher value application field of biomass resource, in particular to a kind of attapulgite-biomass active
Charcoal soil remediation material and preparation method thereof.
Background technique
The development that the higher value application of industrial solid castoff resource has become resource-conserving and environment-friendly society becomes
Gesture.The vegetable seed dregs of fat are a kind of by-products after vegetable seed oil expression, belong to one of biomass industrial solid castoff.According to statistics,
14,000,000 tons of China's rapeseed yield in 2016, this will undoubtedly generate a large amount of vegetable seed dregs of fat solid waste.
Current processing method is these vegetable seed dregs of fat to be used as to vegetable fertilizer, but this does not realize biomass industry
The higher value application of solid waste resource is horizontal.It is carbon source using the vegetable seed dregs of fat, is the high level of vegetable seed dregs of fat solid waste
Change to utilize and opens a new direction, however the easy coking in pyrolytic process of the vegetable seed dregs of fat, it is produced to seriously affect its charing
The specific surface area and pore structure of object.
Summary of the invention
The present invention is intended to provide a kind of attapulgite-activated carbon from activated sludge soil remediation material and preparation method thereof, skill
Art scheme is that it is compound to prepare attapulgite/charcoal using a step high temperature pyrolytic cracking (HTP) first using attapulgite and the vegetable seed dregs of fat as raw material
Then material is handled by acid activation and attapulgite/absorbent charcoal composite material is made.
Specific steps are as follows:
(1) the vegetable seed dregs of fat and attapulgite powder are uniformly mixed, then gained mixture is placed under inert atmosphere hot
Attapulgite/carbon composite is made in solution,
Wherein, the mass ratio of the vegetable seed dregs of fat and attapulgite powder is 0.5~3:1,
Inert atmosphere is nitrogen, be pyrolyzed be 450~650 DEG C under the conditions of react 2~5 hours；
(2) the resulting attapulgite/carbon composite of step (1) is added in acid solution and carries out hydro-thermal process, i.e.,
Attapulgite/absorbent charcoal composite material is made,
Wherein, the mass ratio of attapulgite/carbon composite and acid solution be 0.1~0.3:1, acid solution be hydrogen from
Sub- concentration is hydrochloric acid solution, sulfuric acid solution or the nitric acid solution of 3~10 mol/Ls,
Hydro-thermal process is hydro-thermal reaction 6~12 hours under the conditions of 150~180 DEG C.
The beneficial effects of the present invention are:
1, the present invention is based on protein and amino acid abundant in the cereal and oil industry solid waste vegetable seed dregs of fat, using its work
The nitrogen and phosphorus element for being rich in raw material itself for the active carbon that organic carbon source is prepared is formed by active group, to be conducive to
Heavy metal ion in curing soil avoids this pollution of part heavy metal to soil ambient enviroment；
2,1-dimention nano attapulgite is added in the present invention in vegetable seed dregs of fat pyrolytic process, using a step high temperature pyrolysis legal system
When standby attapulgite/carbon composite, the coking problem in vegetable seed dregs of fat pyrolytic process can be effectively prevented, to improve activity
The specific surface area of Carbon Materials improves its pore structure；The technique has many advantages, such as low in cost, simple process；
3, the present invention is pyrolyzed using the specific organic carbon source vegetable seed dregs of fat, and the Carbon Materials being converted to are zigzag to be similar to
Pattern is coated on attapulgite surface (as shown in Fig. 1), increases the specific surface area of composite material；
4, the present invention carries out acidification hydro-thermal process to obtained attapulgite/carbon composite, there is 2 aspect effects in this way
Fruit: 1. inorganic acid can activate the active group of charcoal material surface；2. can effectively remove the vegetable seed dregs of fat is pyrolyzed the raw material of wood-charcoal to be formed
Original metal impurities ion in material.This 2 aspect effect is all conducive to enhance suction of the composite material to heavy metal ions in soil
Attached and solidification.
Detailed description of the invention
Fig. 1 is attapulgite/absorbent charcoal composite material TEM figure prepared in the embodiment of the present invention 4.
Specific embodiment
Embodiment 1
1,1.0 kilograms of vegetable seed dregs of fat and 2.0 kilograms of attapulgite powders are uniformly mixed, is then placed in gained mixture
It under nitrogen atmosphere, is pyrolyzed 6 hours under the conditions of temperature is 450 DEG C, attapulgite/carbon composite is made；
2, it takes the resulting attapulgite/carbon composite of 1.0 kilograms of steps 1 to be added to 10.0 kilograms of hydrogen ion concentrations to be
In the hydrochloric acid solution of 3.0 mol/Ls, hydro-thermal process 6 hours under the conditions of temperature is 180 DEG C, it is filtered, washed, dries, obtain
Attapulgite/absorbent charcoal composite material.
Embodiment 2
1,6.0 kilograms of vegetable seed dregs of fat and 2 kilograms of attapulgite powders are uniformly mixed, gained mixture is then placed in nitrogen
It under gas atmosphere, is pyrolyzed 2 hours under the conditions of temperature is 650 DEG C, attapulgite/carbon composite is made；
2, it takes the resulting attapulgite/carbon composite of 2.0 kilograms of steps 1 to be added to 6.7 kilograms of hydrogen ion concentrations to be
In the sulfuric acid solution of 10.0 mol/Ls, hydro-thermal process 12 hours under the conditions of temperature is 150 DEG C, it is filtered, washed, dries, that is, make
Obtain attapulgite/absorbent charcoal composite material.
Embodiment 3
1,3.5 kilograms of vegetable seed dregs of fat and 2.0 kilograms of attapulgite powders are uniformly mixed, is then placed in gained mixture
It under nitrogen atmosphere, is pyrolyzed 4 hours under the conditions of temperature is 550 DEG C, attapulgite/carbon composite is made；
2, taking the resulting attapulgite/carbon composite of 1.0 kilograms of steps 1 to be added to 5.0 kilograms of hydrogen ion concentrations is 6.5
In the nitric acid solution of mol/L, hydro-thermal process 9 hours under the conditions of temperature is 165 DEG C, it is filtered, washed, dries, obtain recessed
Convex stick stone/absorbent charcoal composite material.
Embodiment 4
1,4.0 kilograms of vegetable seed dregs of fat and 2.0 kilograms of attapulgite powders are uniformly mixed, is then placed in gained mixture
It under nitrogen atmosphere, is pyrolyzed 3 hours under the conditions of temperature is 600 DEG C, attapulgite/carbon composite is made；
2, taking the resulting attapulgite/carbon composite of 1.0 kilograms of steps 1 to be added to 4.0 kilograms of hydrogen ion concentrations is 5.0
In the nitric acid solution of mol/L, hydro-thermal process 10 hours under the conditions of temperature is 170 DEG C, it is filtered, washed, dries, obtain recessed
Convex stick stone/absorbent charcoal composite material.
Comparative example 1
Compared to above-described embodiment 4, remove " addition attapulgite powder " this process, other process conditions are constant:
4.0 kilograms of vegetable seed dregs of fat are placed under nitrogen atmosphere, are pyrolyzed 3 hours under the conditions of temperature is 600 DEG C, then by it
It is added in the nitric acid solution that 4.0 kilograms of hydrogen ion concentrations are 5.0 mol/Ls, the hydro-thermal process 10 under the conditions of temperature is 170 DEG C
Hour, it is filtered, washed, dries, obtain absorbent charcoal material.
Comparative example 2
On the basis of comparative example 1, the vegetable seed dregs of fat are replaced with into the equal glucose of phosphorus content, referring to comparative example 1 also into
Row is adequately pyrolyzed and hydro-thermal process.
Comparative example 3
On the basis of comparative example 1, the vegetable seed dregs of fat are replaced with into the equal cellulose of phosphorus content, referring to comparative example 1 also into
Row is adequately pyrolyzed and hydro-thermal process.
Comparative example 4
Compared to above-described embodiment 4, remove " hydro-thermal process " this process, other process conditions are constant:
4.0 kilograms of vegetable seed dregs of fat and 2.0 kilograms of attapulgite powders are uniformly mixed, gained mixture is then placed in nitrogen
It under gas atmosphere, is pyrolyzed 3 hours under the conditions of temperature is 600 DEG C, attapulgite/carbon composite is made.
Soil remediation performance evaluation
Pb and Cd ion in fixed-contamination soil is repaired using chemical passivation method: taking 1.0 kilograms of same contaminated soils,
Attapulgite/absorbent charcoal composite material (5%, mass ratio) obtained by embodiment and comparative example is added to mix with contaminated soil
It is even, under room temperature (25 DEG C), after keeping the 60% of maximum water holding capacity to cultivate 14 days, deionized water elution is added, until elution
Water reaches 10L, and the soil natural eluted is air-dried, and tests and analyzes,
Pedotheque analysis: the soil after reparation and not repaired blank soil are used into 1:1 (molar ratio) HNO3/
H2O2Resolution, and using the heavy metal in atom flame spectrophotometer (AAS) (Jena, Germany, novAA350) measurement digestion solution
Concentration, the content of beary metal after reparation that you can get it or in blank soil,
Heavy metals immobilization rate=(quality of corresponding heavy metal in the quality of heavy metal in soil/blank soil after reparation) ×
100%
Testing result is as follows:
| Pb curing degree | Cd curing degree | |
| Embodiment 1 | 41.5 | 51.6 |
| Embodiment 2 | 42.3 | 54.2 |
| Embodiment 3 | 42.7 | 53.6 |
| Embodiment 4 | 44.7 | 55.8 |
| Comparative example 1 | 29.5 | 37.9 |
| Comparative example 2 | 5.3 | 5.8 |
| Comparative example 3 | 4.6 | 5.0 |
| Comparative example 4 | 27.8 | 32.4 |
Claims (7)
1. a kind of attapulgite-activated carbon from activated sludge soil remediation material, it is characterised in that: the soil remediation material be with
Attapulgite and the vegetable seed dregs of fat are raw material, prepare attapulgite/carbon composite using a step high temperature pyrolytic cracking (HTP) first, then lead to
Made from peracid is activated；
The acid activation processing is that attapulgite/carbon composite is added in acid solution to be lauched in 150~180 DEG C of conditions
Thermal response 6~12 hours.
2. a kind of attapulgite as described in claim 1-activated carbon from activated sludge soil remediation material preparation method, feature
It is: the preparation method is that,
(1) the vegetable seed dregs of fat and attapulgite powder are uniformly mixed, then gained mixture is placed under inert atmosphere and is pyrolyzed, made
Obtain attapulgite/carbon composite；
(2) the resulting attapulgite/carbon composite of step (1) is added in acid solution and carries out hydro-thermal process, obtained
Attapulgite/absorbent charcoal composite material.
3. attapulgite as claimed in claim 2-activated carbon from activated sludge soil remediation material preparation method, feature exist
In: in step (1), the mass ratio of the vegetable seed dregs of fat and attapulgite powder is 0.5~3:1.
4. attapulgite as claimed in claim 2-activated carbon from activated sludge soil remediation material preparation method, feature exist
In: in step (1), be pyrolyzed be 450~650 DEG C under the conditions of react 2~5 hours.
5. attapulgite as claimed in claim 2-activated carbon from activated sludge soil remediation material preparation method, feature exist
In: in step (2), the mass ratio of attapulgite/carbon composite and acid solution is 0.1~0.3:1.
6. attapulgite as claimed in claim 2-activated carbon from activated sludge soil remediation material preparation method, feature exist
In: acid solution described in step (2) is the hydrochloric acid solution, sulfuric acid solution or nitric acid that hydrogen ion concentration is 3~10 mol/Ls
Solution.
7. attapulgite as claimed in claim 2-activated carbon from activated sludge soil remediation material preparation method, feature exist
In: hydro-thermal process described in step (2) is hydro-thermal reaction 6~12 hours under the conditions of 150~180 DEG C.
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| CN108949188A (en) * | 2018-08-02 | 2018-12-07 | 佛山皖阳生物科技有限公司 | A kind of preparation method of antibacterial passivator |
| CN110016355A (en) * | 2019-04-17 | 2019-07-16 | 南京三聚生物质新材料科技有限公司 | A kind of biomass carbonated method and utilize soil conditioner made from this method |
| CN110156012B (en) * | 2019-06-04 | 2020-12-25 | 北方民族大学 | Activated carbon and method for preparing activated carbon by using waste edible oil |
| CN111019404A (en) * | 2019-11-29 | 2020-04-17 | 淮阴工学院 | Modified attapulgite for rubber reinforcement and preparation method thereof |
| CN110947364A (en) * | 2019-12-12 | 2020-04-03 | 甘肃农业大学 | Heavy metal contaminated soil remediation agent and application thereof |
| CN111004069A (en) * | 2019-12-31 | 2020-04-14 | 群发(广东)生物科技有限公司 | Method for preparing novel organic fertilizer |
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