CN109967516A - A kind of method that intensified petroleum contaminative soil pyrolysis is repaired - Google Patents
A kind of method that intensified petroleum contaminative soil pyrolysis is repaired Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09C—RECLAMATION OF CONTAMINATED SOIL
- B09C1/00—Reclamation of contaminated soil
- B09C1/06—Reclamation of contaminated soil thermally
- B09C1/065—Reclamation of contaminated soil thermally by pyrolysis
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Abstract
The present invention relates to technical field of soil remediation, and in particular to a kind of method that intensified petroleum contaminative soil pyrolysis is repaired, the method use Fe2O3Strengthen pyrolysis remedying oil-polluted soils, has the advantages that environmental protection, low energy consumption, contaminant removal efficiency is high, resource recycling can be achieved.
Description
Technical field
The present invention relates to technical field of soil remediation, and in particular to a kind of side that intensified petroleum contaminative soil pyrolysis is repaired
Method.
Background technique
The important environmental basis that soil is depended on for existence as the mankind, animals and plants and microorganism is nature matter and energy
Participate in the important place of the cyclic processes such as conversion, migration and accumulation.However, soil issues are increasingly with the development of modern civilization
It is prominent." the national Soil Pollution Investigation bulletin " display issued according to Environmental Protection Department and Ministry of Land and Resources, China's soil
Total exceeding standard rate is up to 16.1%.Wherein organic pollutant, especially petroleum pollution, which have become, leads to soil safety problem
One of key factor.In China, the petroleum in environment is entered there are about 600,000 tons via various approach every year, leads to about 500
Ten thousand hm2Soil receive oil pollution, cause incalculable damage.
After petroleum enters soil, it can constantly be adsorbed, decompose, move by processes such as the physics, chemistry and biology of soil
It moves or is detained, cause the variation of soil physico-chemical property, influence plant physiological ecology, change structure of soil microbial community, simultaneously
The surrounding mediums such as big gas and water can also be influenced by the approach such as volatilizing, migrating downward into, and then threaten the health of the mankind.Oil pollution
The component of object is sufficiently complex, especially the macromolecular substances such as aromatic hydrocarbon, colloid and asphalitine, to the reparation of oil-polluted soils
Bring certain difficulty.
Currently, the recovery technique for oil-polluted soils mainly has biological prosthetic, elution and heat treatment technics etc..Biology
Reparation has many advantages, such as that easy to operate, expense is low and secondary pollution is small, but it is only capable of processing low concentration oil-polluted soils and place
The reason period is long, cannot effectively degrade to the heavy crudes such as resin and asphalt component；There are leacheates to separate with soil for elution method
It is difficult, be difficult to adapt to clayed soil and leacheate needs the shortcomings that being further processed.Heat treatment technics has remediation efficiency high, right
The type and concentration adaptability of organic contaminants in soil wait well significant advantages, are answered extensively in oil-polluted soils reparation
With.However, that there are energy consumptions is high, influences the problems such as big to soil physico-chemical property for incineration technology in heat treatment technics, it is current oil
Facing challenges are repaired in contaminated soil heat treatment.Pyrolytic technique can incite somebody to action at relatively low temperature and anaerobic or anaerobic environment
Mink cell focus (resin and asphalt etc.) pyrolysis is the light oil of volatilizable removal and the coke species of nonhazardous, with incineration technology
It compares, pyrolytic technique can save the energy consumption of 40-60%.
Vidonish et al. is in " Pyrolytic treatment and fertility enhancement of soils
contaminated with heavy hydrocarbons.Environ.Sci.Technol.2016,50(5),2498-
It is disclosed in 2506. " and pyrolysis reparation has been carried out to oil-polluted soils using slow pyrolysis, Li Dechang et al. exists
“Remediation ofPetroleum-Contaminated Soil and Simultaneous Recovery ofOil by
2018,52 (9): Fast Pyrolysis.Environmental Science&Technology discloses utilization in 5330. "
Fast pyrogenation has carried out pyrolysis to oil-polluted soils and has repaired, the results showed that pyrolytic technique can be effectively removed oil pollution soil
Total petroleum hydrocarbon substance in earth, but be pyrolyzed to repair and still have the disadvantages of pyrolysis temperature is high, pyrolysis time is long, energy consumption is high.
Chinese patent application CN201710189064.4 discloses a kind of hot restorative procedure of organic polluted soil, uses combustion furnace
Flue gas original position or dystopy heat organic polluted soil, make heavy metal classes pollution, pesticide pollution, hydrocarbon contamination, biology, nutrition
Class pollution is separated from soil, and wherein hydrocarbons pollutant includes petroleum hydrocarbon, halogenated hydrocarbons, polycyclic aromatic hydrocarbon etc., the hot restorative procedure of dystopy
The following steps are included: passing through the hot fume of burner supply by the contaminated soil after screening by being sent into heating furnace at the top of heating furnace
With discharge flue gas in wind mixed chamber's mixing of heating furnace bottom, reaches requirement temperature, contaminated soil is heated, it will be in contaminated soil
Organic pollutant is gradually desorbed and decomposes, and to achieve the purpose that soil sanitation, treated soil is by heating furnace bottom discharging mouth
Discharge.This method has higher pyrolysis effect to hydrocarbons pollutant, but needs to provide the flue gas of combustion furnace, and energy consumption is high, after reaction
It also needs to handle flue gas.
Therefore, the restorative procedure for developing a kind of oil-polluted soils that can solve above-mentioned technical problem is very important.
Summary of the invention
There is provided the purpose of the present invention is overcome the deficiencies in the prior art it is a kind of environmental protection, low energy consumption, contaminant removal efficiency
The restorative procedure of oil-polluted soils high, that resource recycling can be achieved.
The present invention is achieved by the following technical programs:
A kind of method that intensified petroleum contaminative soil pyrolysis is repaired, the method use Fe2O3Strengthen pyrolysis and repairs petroleum wastewater
Contaminate soil.
Preferably, the above method includes the following steps:
(1) oil-polluted soils are dry, crushing, obtains substance A, spare；
(2) by substance A and Fe2O3Mixing, obtains substance B；
(3) substance B is pyrolyzed under anaerobic or anoxia condition.
It is highly preferred that it is natural air drying or heat drying that oil-polluted soils described in step (1) are dry.
It is highly preferred that oil-polluted soils described in step (1) are crushed to 15-40 mesh.
It is highly preferred that Fe described in step (2)2O3Mass ratio with substance A is 0.1-10%.
It is highly preferred that Fe described in step (2)2O3Mass ratio with substance A is 1-5%.
It is highly preferred that anaerobic described in step (3) or anoxia condition are by being continually fed into inert gas in reaction process
It realizes.
It is highly preferred that anaerobic described in step (3) or anoxia condition are by being continually fed into before reacting and in reaction process
What inert gas was realized.
It is highly preferred that inert gas described in step (3) is one or both of nitrogen or argon gas.
It is highly preferred that the flow velocity for being continually fed into inert gas before the reaction is 0.5-2L/min, being passed through the time is 5-
15min。
It is highly preferred that the flow velocity for being continually fed into inert gas in the reaction process is 1-2L/min.
It is highly preferred that pyrolysis temperature described in step (3) is 350-450 DEG C, pyrolysis time 10-120min.
It is highly preferred that pyrolysis temperature described in step (3) is 350-400 DEG C.
It is highly preferred that in substance B pyrolytic process described in step (3), using the stone of indirect condensing method recycling pyrolysis devolatilization
Oil absorbs incondensible tail gas with organic solvent.
It is highly preferred that organic solvent described in step (3) is one or both of n-hexane, acetone.
It is highly preferred that substance B pyrolytic process described in step (3) is in the Equipment for Heating Processing for being equipped with feed inlet and gas outlet
It carries out.
It is highly preferred that Equipment for Heating Processing described in step (3) is tube furnace or rotary kiln.
The beneficial effects of the present invention are:
The present invention only adds Fe2O3Rehabilitating soil, raw material is simple and easy to get, and used Fe2O3It is that soil itself contains
Substance, tail gas is recycled with organic solvent after the completion of pyrolytic reaction, and pollution-free substance generates, Fe harmless to soil2O3It is cheap and
Source is wide.
Fe of the present invention2O3The energy barrier that can reduce pyrolytic reaction makes pyrolytic reaction at relatively low temperature
Start and accelerate the reaction, improve the removal efficiency of petroleum pollution, shorten the pyrolytic reaction time, reduces reaction energy
Consumption, and the destruction of soil physico-chemical property is avoided, the ecological functions of soil are protected, the growth of crops is more advantageous to.
The Fe that the present invention passes through addition certain content2O3, the pyrolysis repairing effect of oil-polluted soils is enhanced, is improved
It is pyrolyzed efficiency, and by control pyrolysis temperature, shortens pyrolysis time, can reach fine at relatively low temperature
Repairing effect.
By Fe2O3The petroleum generated when strengthening pyrolysis remedying oil-polluted soils is recycled, in discovery pyrolysis repair process
The impurity contents such as heavy metal and sulphur are reduced in generated petroleum, and viscosity reduces, and oil quality is promoted, and realize petroleum resources
It recycles.
The method of rehabilitating soil of the present invention is simple and easy, applied widely, the popularization repaired for oil-polluted soils pyrolysis
Scientific basis and theory support are provided with application.
Detailed description of the invention
The SEM figure of soil after soil and embodiment 5 are repaired after Fig. 1 is pollution-free soil, contaminated soil, comparative example 1 are repaired.
(a) it indicates pollution-free soil, (b) indicates contaminated soil, (c) indicate soil after the reparation of comparative example 1, (d) indicate that embodiment 5 is repaired
Soil afterwards.
Wheat hair in soil after soil and embodiment 5 are repaired after Fig. 2 is pollution-free soil, contaminated soil, comparative example 1 are repaired
Bud rate curve graph.
Specific embodiment
The invention will now be further described with reference to specific embodiments, the advantages and features of the present invention will be with description and
It is apparent.But examples are merely exemplary for these, and it is not intended to limit the scope of the present invention in any way.Those skilled in the art
Member it should be understood that without departing from the spirit and scope of the invention can details to technical solution of the present invention and form into
Row modifications or substitutions, but these modifications and replacement are fallen within the protection scope of the present invention.
Embodiment 1
A kind of method that intensified petroleum contaminative soil pyrolysis is repaired:
(1) 15g oil-polluted soils are subjected to natural air drying, removal bulk rubble, the impurity such as plant and animal residues, crush and
15 meshes are crossed, substance A is obtained, it is spare；
(2) by substance A and 0.03g Fe2O3It is sufficiently mixed, obtains substance B；
(3) substance B is put into pyrolytic reaction slot, and pyrolytic reaction slot is put into tube furnace, continued in reaction process
It is passed through nitrogen, nitrogen flow rate 1L/min, setting heat treatment temperature is 350 DEG C, heat treatment time 120min, in reaction process
Using the petroleum of indirect condensing method recycling pyrolysis devolatilization, incondensible tail gas finally is absorbed with the absorption bottle equipped with n-hexane,
After the reaction was completed, cooled to room temperature to get.
Embodiment 2
A kind of method that intensified petroleum contaminative soil pyrolysis is repaired:
(1) 15g oil-polluted soils are subjected to natural air drying, removal bulk rubble, the impurity such as plant and animal residues, crush and
40 meshes are crossed, substance A is obtained, it is spare；
(2) by substance A and 0.3g Fe2O3It is sufficiently mixed, obtains substance B；
(3) substance B is put into pyrolytic reaction slot, and pyrolytic reaction slot is put into rotary kiln, before reaction and reacted
Nitrogen is continually fed into journey, nitrogen flow rate is 0.5L/min before reacting, and being passed through the time is 15min, nitrogen flow rate in reaction process
For 2L/min, it is 450 DEG C, heat treatment time 10min that heat treatment temperature, which is arranged, is recycled in reaction process using indirect condensing method
The petroleum of pyrolysis devolatilization finally absorbs incondensible tail gas, after the reaction was completed, natural cooling with the absorption bottle equipped with n-hexane
To room temperature to get.
Embodiment 3
A kind of method that intensified petroleum contaminative soil pyrolysis is repaired:
(1) 15g oil-polluted soils are subjected to natural air drying, removal bulk rubble, the impurity such as plant and animal residues, crush and
25 meshes are crossed, substance A is obtained, it is spare；
(2) by substance A and 1.5g Fe2O3It is sufficiently mixed, obtains substance B；
(3) substance B is put into pyrolytic reaction slot, and pyrolytic reaction slot is put into tube furnace, before reaction and reacted
Nitrogen is continually fed into journey, nitrogen flow rate is 2L/min before reacting, and being passed through the time is 5min, and nitrogen flow rate is in reaction process
1.5L/min, setting heat treatment temperature are 400 DEG C, heat treatment time 60min, are recycled in reaction process using indirect condensing method
The petroleum of pyrolysis devolatilization finally absorbs incondensible tail gas with the absorption bottle equipped with acetone and naturally cools to after the reaction was completed
Room temperature to get.
Embodiment 4
A kind of method that intensified petroleum contaminative soil pyrolysis is repaired:
(1) 15g oil-polluted soils are subjected to natural air drying, removal bulk rubble, the impurity such as plant and animal residues, crush and
30 meshes are crossed, substance A is obtained, it is spare；
(2) by substance A and 0.15g Fe2O3It is sufficiently mixed, obtains substance B；
(3) substance B is put into pyrolytic reaction slot, and pyrolytic reaction slot is put into rotary kiln, before reaction and reacted
Nitrogen is continually fed into journey, nitrogen flow rate is 1.5L/min before reacting, and being passed through the time is 10min, nitrogen flow rate in reaction process
For 1.2L/min, it is 380 DEG C, heat treatment time 80min that heat treatment temperature, which is arranged, is returned in reaction process using indirect condensing method
The petroleum of pyrolysis devolatilization is received, finally absorbs incondensible tail gas, after the reaction was completed, natural cooling with the absorption bottle equipped with acetone
To room temperature to get.
Embodiment 5
A kind of method that intensified petroleum contaminative soil pyrolysis is repaired:
(1) 15g oil-polluted soils are subjected to natural air drying, removal bulk rubble, the impurity such as plant and animal residues, crush and
24 meshes are crossed, substance A is obtained, it is spare；
(2) by substance A and 0.75g Fe2O3It is sufficiently mixed, obtains substance B；
(3) substance B is put into pyrolytic reaction slot, and pyrolytic reaction slot is put into tube furnace, before reaction and reacted
Nitrogen is continually fed into journey, nitrogen flow rate is 1L/min before reacting, and being passed through the time is 10min, and nitrogen flow rate is in reaction process
1L/min, setting heat treatment temperature are 400 DEG C, heat treatment time 30min, using indirect condensing method recycling heat in reaction process
The petroleum of volatilization is solved, finally incondensible tail gas is absorbed with the absorption bottle equipped with acetone and naturally cools to room after the reaction was completed
Temperature to get.
Comparative example 1
The difference of method and embodiment 5 that a kind of pyrolysis of intensified petroleum contaminative soil is repaired, which is only that, does not add Fe2O3,
Other conditions are all the same, specific as follows:
(1) 15g oil-polluted soils are subjected to natural air drying, removal bulk rubble, the impurity such as plant and animal residues, crush and
24 meshes are crossed, substance A is obtained, it is spare；
(2) substance A is put into pyrolytic reaction slot, and pyrolytic reaction slot is put into tube furnace, before reaction and reacted
Nitrogen is continually fed into journey, nitrogen flow rate is 1L/min before reacting, and being passed through the time is 10min, and nitrogen flow rate is in reaction process
1L/min, setting heat treatment temperature are 400 DEG C, heat treatment time 30min, using indirect condensing method recycling heat in reaction process
The petroleum of volatilization is solved, finally incondensible tail gas is absorbed with the absorption bottle equipped with acetone and naturally cools to room after the reaction was completed
Temperature to get.
Comparative example 2
The difference of method and embodiment 5 that a kind of pyrolysis of intensified petroleum contaminative soil is repaired is only that pyrolysis temperature is 600
DEG C, other conditions are all the same, specific as follows:
(1) 15g oil-polluted soils are subjected to natural air drying, removal bulk rubble, the impurity such as plant and animal residues, crush and
24 meshes are crossed, substance A is obtained, it is spare；
(2) by substance A and 0.75g Fe2O3It is sufficiently mixed, obtains substance B；
(3) substance B is put into pyrolytic reaction slot, and pyrolytic reaction slot is put into tube furnace, before reaction and reacted
Nitrogen is continually fed into journey, nitrogen flow rate is 1L/min before reacting, and being passed through the time is 10min, and nitrogen flow rate is in reaction process
1L/min, setting heat treatment temperature are 600 DEG C, heat treatment time 30min, using indirect condensing method recycling heat in reaction process
The petroleum of volatilization is solved, finally incondensible tail gas is absorbed with the absorption bottle equipped with acetone and naturally cools to room after the reaction was completed
Temperature to get.
Test case 1
Total petroleum of soil after being repaired using USA EPA Method 3550 method testing example 1-5 and comparative example 1-2
The removal rate of hydrocarbon, the results are shown in Table 1.
The total petroleum hydrocarbon removal rate of soil after table 1 is repaired
| Sample | Total petroleum hydrocarbon removal rate/% |
| Embodiment 1 | 90.47 |
| Embodiment 2 | 91.45 |
| Embodiment 3 | 100 |
| Embodiment 4 | 90.52 |
| Embodiment 5 | 95.80 |
| Comparative example 1 | 70.27 |
| Comparative example 2 | 100 |
Test case 2
Soil after pollution-free soil, contaminated soil, embodiment 1, embodiment 3, embodiment 5 and comparative example 1-2 are repaired
Wheat germination rate experiment is carried out, full grains, wheat seed 700 of health is selected, is randomly divided into 7 groups, every group 100,
It is even to be spread on 7 pollution-free soil containing phase homogenous quantities, contaminated soil, embodiment 1, embodiment 3, embodiment 5 and comparative example 1-2
After reparation in the identical glass culture dish of the size of soil.7 culture dishes are placed in growth cabinet, specific retesion of soil is kept
It is 60%, when regulating thermostatic case sunshine a length of 16 hours, the temperature of day/night is 26/22 DEG C, air humidity 70%,
Wheat germination situation is observed, until there is no wheat germinations, measurement wheat germination rate, the results are shown in Table 2.
The wheat germination rate test result of 2 soil of table
| Sample | Wheat germination rate/% |
| Embodiment 1 | 70 |
| Embodiment 3 | 72 |
| Embodiment 5 | 76 |
| Comparative example 1 | 61 |
| Comparative example 2 | 52 |
| Pollution-free soil | 68 |
| Contaminated soil | 28 |
As shown in Table 2, Fe2O3After soil wheat germination rate after strengthening pyrolysis reparation is significantly higher than comparative example 1-2 reparation
Soil, even better than pollution-free soil, this is because Fe2O3Strengthen the stone that the soil surface after pyrolysis is repaired forms one layer of black
Black carbonizable substance film, the film surface have a large amount of small holes, accelerate the transmission of nutriment and moisture, be more advantageous to
The growth of plant.
The technical means disclosed in the embodiments of the present invention is not limited to the technical means disclosed in the above technical means, and further includes
Technical solution consisting of any combination of the above technical features.The foregoing is a specific embodiment of the present invention, should refer to
Out, for those skilled in the art, without departing from the principle of the present invention, can also make several
Improvements and modifications, these modifications and embellishments are also considered to be within the scope of the present invention.
Claims (10)
1. a kind of method that intensified petroleum contaminative soil pyrolysis is repaired, which is characterized in that the method uses Fe2O3Strengthen pyrolysis
Remedying oil-polluted soils.
2. restorative procedure according to claim 1, which comprises the steps of:
(1) oil-polluted soils are dry, crushing, obtains substance A, spare；
(2) by substance A and Fe2O3Mixing, obtains substance B；
(3) substance B is pyrolyzed under anaerobic or anoxia condition.
3. restorative procedure according to claim 2, which is characterized in that oil-polluted soils described in step (1) are crushed to
15-40 mesh.
4. restorative procedure according to claim 2, which is characterized in that Fe described in step (2)2O3With the mass ratio of substance A
For 0.1-10%.
5. restorative procedure according to claim 2, which is characterized in that anaerobic described in step (3) or anoxia condition are logical
It crosses in reaction process and is continually fed into inert gas realization.
6. restorative procedure according to claim 5, which is characterized in that anaerobic described in step (3) or anoxia condition are logical
Cross before reaction and be continually fed into reaction process inert gas realization.
7. restorative procedure according to claim 6, which is characterized in that be continually fed into the flow velocity of inert gas before the reaction
For 0.5-2L/min, being passed through the time is 5-15min, and the flow velocity that inert gas is continually fed into reaction process is 1-2L/min.
8. restorative procedure according to claim 2, which is characterized in that pyrolysis temperature described in step (3) is 350-450
DEG C, pyrolysis time 10-120min.
9. restorative procedure according to claim 8, which is characterized in that pyrolysis temperature described in step (3) is preferably 350-
400℃。
10. restorative procedure according to claim 2, which is characterized in that in substance B pyrolytic process described in step (3), adopt
With the petroleum of indirect condensing method recycling pyrolysis devolatilization, incondensible tail gas is absorbed with organic solvent.
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| CN111822492A (en) * | 2020-07-30 | 2020-10-27 | 广东佳德环保科技有限公司 | Device system and method for treating petroleum-polluted soil |
| CN112536317A (en) * | 2020-11-17 | 2021-03-23 | 武汉大学 | Cadmium-polluted soil remediation method based on biomass co-pyrolysis |
| WO2021227361A1 (en) * | 2020-05-09 | 2021-11-18 | 中国石油大学(华东) | Combined treatment method for petroleum contaminated soil |
| CN113732036A (en) * | 2021-08-24 | 2021-12-03 | 中国环境科学研究院 | Method for promoting thermal treatment restoration of heavy petroleum polluted soil |
| CN115646443A (en) * | 2022-10-25 | 2023-01-31 | 常州大学 | Method for preparing efficient heavy metal adsorption material by co-pyrolysis of petroleum-polluted soil and ferric salt and application of heavy metal wastewater treatment |
| CN116274323A (en) * | 2021-12-20 | 2023-06-23 | 中国石油天然气集团有限公司 | Method and system for treating oil-contaminated soil and related application |
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| WO2021227361A1 (en) * | 2020-05-09 | 2021-11-18 | 中国石油大学(华东) | Combined treatment method for petroleum contaminated soil |
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| CN112536317A (en) * | 2020-11-17 | 2021-03-23 | 武汉大学 | Cadmium-polluted soil remediation method based on biomass co-pyrolysis |
| CN113732036A (en) * | 2021-08-24 | 2021-12-03 | 中国环境科学研究院 | Method for promoting thermal treatment restoration of heavy petroleum polluted soil |
| CN113732036B (en) * | 2021-08-24 | 2023-10-20 | 中国环境科学研究院 | Method for promoting heat treatment and restoration of heavy petroleum polluted soil |
| CN116274323A (en) * | 2021-12-20 | 2023-06-23 | 中国石油天然气集团有限公司 | Method and system for treating oil-contaminated soil and related application |
| CN115646443A (en) * | 2022-10-25 | 2023-01-31 | 常州大学 | Method for preparing efficient heavy metal adsorption material by co-pyrolysis of petroleum-polluted soil and ferric salt and application of heavy metal wastewater treatment |
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Application publication date: 20190705 |