CN106947486A - 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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- CN106947486A CN106947486A CN201710239445.9A CN201710239445A CN106947486A CN 106947486 A CN106947486 A CN 106947486A CN 201710239445 A CN201710239445 A CN 201710239445A CN 106947486 A CN106947486 A CN 106947486A
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- attapulgite
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- 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
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Abstract
The invention belongs to the higher value application field of biomass resource, more particularly 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, obtained attapulgite/absorbent charcoal composite material is then handled by acid activation.
Description
Technical field
The invention belongs to the higher value application field of biomass resource, more particularly to a kind of attapulgite-biomass active
Charcoal soil remediation material and preparation method thereof.
Background technology
The development as resource-conserving and environment-friendly society becomes the higher value application of industrial solid castoff resource
Gesture.The vegetable seed dregs of fat are a kind of accessory substance after vegetable seed oil expression, the one kind belonged in biomass industrial solid castoff.According to statistics,
14,000,000 tons of China's rapeseed yield in 2016, this will undoubtedly produce a large amount of vegetable seed dregs of fat solid waste.
Current processing method is that these vegetable seed dregs of fat are used as into vegetable fertilizer, but this does not realize biomass industry
The higher value application level of solid waste resource.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 open a new direction, but the easy coking in pyrolytic process of the vegetable seed dregs of fat, so as to have a strong impact on its charing production
The specific surface area and pore structure of thing.
The content 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, its skill
Art scheme is, using attapulgite and the vegetable seed dregs of fat as raw material, to prepare attapulgite/charcoal using a step high temperature pyrolytic cracking (HTP) first and be combined
Material, is then handled by acid activation and attapulgite/absorbent charcoal composite material is made.
Concretely comprise the following steps：
(1) the vegetable seed dregs of fat and attapulgite powder are uniformly mixed, then gained mixture is placed under inert atmosphere hot
Solution, is made attapulgite/carbon composite,
Wherein, the vegetable seed dregs of fat and the mass ratio of attapulgite powder are 0.5~3:1,
Inert atmosphere is nitrogen, is pyrolyzed to react 2~5 hours under the conditions of 450~650 DEG C；
(2) attapulgite/carbon composite obtained by 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 is 0.1~0.3:1, acid solution be hydrogen from
Sub- concentration is hydrochloric acid solution, sulfuric acid solution or the salpeter 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：
1st, the present invention is based on the protein and amino acid enriched in the cereal and oil industry solid waste vegetable seed dregs of fat, using its work
The active group that the activated carbon prepared by organic carbon source has been rich in the nitrogen of raw material itself, P elements are formed, so as to be conducive to
Heavy metal ion in curing soil, it is to avoid this pollution of part heavy metal to soil surrounding environment；
2nd, the present invention adds 1-dimention nano attapulgite in vegetable seed dregs of fat pyrolytic process, using a step high temperature pyrolysis legal system
During standby attapulgite/carbon composite, the coking problem in vegetable seed dregs of fat pyrolytic process can be effectively prevented, so as to improve activity
The specific surface area of Carbon Materials, improves its pore structure；The technique has the advantages that with low cost, technique is simple；
3rd, the present invention is using the pyrolysis of the specific organic carbon source vegetable seed dregs of fat, and the Carbon Materials changed into are with similar to zigzag
Pattern is coated on attapulgite surface (as shown in Figure 1), increases the specific surface area of composite；
4th, the present invention carries out acidifying hydro-thermal process to obtained attapulgite/carbon composite, so there is 2 aspect effects
Really：1. inorganic acid can activate the active group of charcoal material surface；2. the vegetable seed dregs of fat can effectively be removed and be pyrolyzed the raw material of wood-charcoal to be formed
Original metal impurities ion in material.This 2 aspect effect is all conducive to strengthening suction of the composite to heavy metal in soil ion
Attached and solidification.
Brief description of the drawings
Fig. 1 schemes for the TEM of attapulgite/absorbent charcoal composite material prepared in the embodiment of the present invention 4.
Embodiment
Embodiment 1
1st, 1.0 kilograms of vegetable seed dregs of fat and 2.0 kilograms of attapulgite powders are uniformly mixed, are then placed in gained mixture
Under nitrogen atmosphere, it is pyrolyzed 6 hours under the conditions of temperature is 450 DEG C, attapulgite/carbon composite is made；
2nd, take attapulgite/carbon composite obtained by 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, the hydro-thermal process 6 hours under the conditions of temperature is 180 DEG C is filtered, washs, dried, that is, is made
Attapulgite/absorbent charcoal composite material.
Embodiment 2
1st, 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
Under gas atmosphere, it is pyrolyzed 2 hours under the conditions of temperature is 650 DEG C, attapulgite/carbon composite is made；
2nd, take attapulgite/carbon composite obtained by 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, the hydro-thermal process 12 hours under the conditions of temperature is 150 DEG C is filtered, washs, dried, that is, makes
Obtain attapulgite/absorbent charcoal composite material.
Embodiment 3
1st, 3.5 kilograms of vegetable seed dregs of fat and 2.0 kilograms of attapulgite powders are uniformly mixed, are then placed in gained mixture
Under nitrogen atmosphere, it is pyrolyzed 4 hours under the conditions of temperature is 550 DEG C, attapulgite/carbon composite is made；
2nd, it is 6.5 to take attapulgite/carbon composite obtained by 1.0 kilograms of steps 1 to be added to 5.0 kilograms of hydrogen ion concentrations
In the salpeter solution of mol/L, the hydro-thermal process 9 hours under the conditions of temperature is 165 DEG C filters, washs, dried, that is, is made recessed
Convex rod stone/absorbent charcoal composite material.
Embodiment 4
1st, 4.0 kilograms of vegetable seed dregs of fat and 2.0 kilograms of attapulgite powders are uniformly mixed, are then placed in gained mixture
Under nitrogen atmosphere, it is pyrolyzed 3 hours under the conditions of temperature is 600 DEG C, attapulgite/carbon composite is made；
2nd, it is 5.0 to take attapulgite/carbon composite obtained by 1.0 kilograms of steps 1 to be added to 4.0 kilograms of hydrogen ion concentrations
In the salpeter solution of mol/L, the hydro-thermal process 10 hours under the conditions of temperature is 170 DEG C filters, washs, dried, that is, is made recessed
Convex rod 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 salpeter 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, filtering, washing, dry, i.e., obtained 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, also entered with reference to comparative example 1
Row is sufficiently 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, also entered with reference to comparative example 1
Row is sufficiently 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
Under gas atmosphere, it 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 ions in fixed-contamination soil are repaired using chemical passivation method：1.0 kilograms of same contaminated soils are taken,
Attapulgite/absorbent charcoal composite material (5%, mass ratio) obtained by addition embodiment and comparative example is mixed with contaminated soil
It is even, under room temperature (25 DEG C), after the 60% of holding maximum water holding capacity cultivates 14 days, deionized water elution is added, until eluting
Water reaches 10L, and the soil natural eluted is air-dried, and tests and analyzes,
Pedotheque is analyzed：Soil after reparation and not repaired blank soil are used 1:1 (mol ratio) HNO3/
H2O2Clear up, and the heavy metal in digestion solution is determined using atom flame spectrophotometer (AAS) (Jena, Germany, novAA350)
Concentration, you can draw the content of beary metal after repairing 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 such as following table：
| Pb curing degrees | Cd curing degrees | |
| 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：Described soil remediation material be with
Attapulgite and the vegetable seed dregs of fat are raw material, prepare attapulgite/carbon composite, Ran Houtong using a step high temperature pyrolytic cracking (HTP) first
Made from peracid activation process.
2. a kind of preparation method of attapulgite as claimed in claim 1-activated carbon from activated sludge soil remediation material, its feature
It is：The preparation method is,
(1) the vegetable seed dregs of fat and attapulgite powder are uniformly mixed, then gained mixture is placed under inert atmosphere and is pyrolyzed, system
Obtain attapulgite/carbon composite；
(2) attapulgite/carbon composite obtained by step (1) is added in acid solution and carries out hydro-thermal process, that is, be made
Attapulgite/absorbent charcoal composite material.
3. the preparation method of attapulgite as claimed in claim 2-activated carbon from activated sludge soil remediation material, its feature exists
In：In step (1), the vegetable seed dregs of fat are 0.5~3 with the mass ratio of attapulgite powder:1.
4. the preparation method of attapulgite as claimed in claim 2-activated carbon from activated sludge soil remediation material, its feature exists
In：In step (1), it is pyrolyzed to react 2~5 hours under the conditions of 450~650 DEG C.
5. the preparation method of attapulgite as claimed in claim 2-activated carbon from activated sludge soil remediation material, its feature exists
In：In step (2), the mass ratio of attapulgite/carbon composite and acid solution is 0.1~0.3:1.
6. the preparation method of attapulgite as claimed in claim 2-activated carbon from activated sludge soil remediation material, its feature exists
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. the preparation method of attapulgite as claimed in claim 2-activated carbon from activated sludge soil remediation material, its feature exists
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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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN110156012A (en) * | 2019-06-04 | 2019-08-23 | 北方民族大学 | Active carbon and the method for preparing active carbon using recycled wood materials |
| 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 |
| CN111019404A (en) * | 2019-11-29 | 2020-04-17 | 淮阴工学院 | Modified attapulgite for rubber reinforcement and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN110156012A (en) * | 2019-06-04 | 2019-08-23 | 北方民族大学 | Active carbon and the method for preparing active carbon using recycled wood materials |
| 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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