CN108786725A - A kind of preparation method of biological carbon for rehabilitating soil environment - Google Patents
A kind of preparation method of biological carbon for rehabilitating soil environment Download PDFInfo
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- CN108786725A CN108786725A CN201810505222.7A CN201810505222A CN108786725A CN 108786725 A CN108786725 A CN 108786725A CN 201810505222 A CN201810505222 A CN 201810505222A CN 108786725 A CN108786725 A CN 108786725A
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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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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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
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
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Abstract
The invention discloses a kind of preparation methods of the biological carbon for rehabilitating soil environment, include the following steps：（1）Stalk pretreatment,（2）High temperature high pressure process,（3）Immersion treatment,（4）Modifying process,（5）Carbonization treatment.The present invention provides a kind of preparation methods of biological carbon, integrated artistic specification, process collocation is reasonable, the large specific surface area of biological carbon obtained, adsorption capacity is strong, it is strong to the adsorption capacity of the harmful elements ingredients such as heavy metal in soil, safety of soil environment, great application value can be obviously improved.
Description
Technical field
The invention belongs to biological carbon processing and manufacturing technologies, and in particular to a kind of biological carbon for rehabilitating soil environment
Preparation method.
Background technology
Agricultural crop straw is the general name of ripe crops stem and leaf part.Be often referred to wheat, rice, corn, potato, rape,
The remainder of cotton, sugarcane and other crops after harvesting seed.The photosynthetic product of crops has more than half to deposit
It is in stalk, for stalk rich in carbon, nitrogen, phosphorus, potassium, calcium, magnesium and organic matter etc., being one kind having multiduty reproducible biology
Resource.Existing a part of agricultural crop straw is used in the making of biological carbon.
With the development of industry, the chemical industry such as many heavy metals endanger ingredient and are penetrated into soil by water source, these are harmful
Ingredient has seriously affected the growth of crops, gently then leads to crop failure, heavy then crop is made to be enriched a large amount of harmful element
Ingredient, and then affect the health of human body.In this regard, people need to carry out contaminated soil the reparation of quality.Wherein with regard to someone
Biological carbon made of agricultural crop straw is made an addition in soil and is adsorbed, even removal harmful components are reduced, although playing
Good effect, but the problems such as there are still adsorption efficiency and not satisfactory effects.
Invention content
The purpose of the present invention is for existing problem, provide a kind of preparation of the biological carbon for rehabilitating soil environment
Method.
The present invention is achieved by the following technical solutions：
A kind of preparation method of biological carbon for rehabilitating soil environment, includes the following steps：
（1）Stalk pretreatment：
Stalk cleaned up with clear water after drying, then put into pulverizer and crush processing, smashes it through 80 mesh
It is spare to obtain straw powder；
（2）High temperature high pressure process：
By step（1）The straw powder of gained is put into vapor tight tank, is passed through high-temperature vapor into vapor tight tank, while by vapor tight tank
Interior pressure increases to 0.5 ~ 0.55MPa, and heat-insulation pressure keeping is quickly unloaded again after handling 20 ~ 24min to normal temperature and pressure, finally by straw powder
It takes out spare；
（3）Immersion treatment：
By step（2）Treated, and straw powder is immersed in citric acid solution, is taken out after 8 ~ 10min of immersion treatment, is used deionization
Water is spare after rinsing one time；
（4）Modifying process：
A. argon gas is passed through into reaction kettle, then by methyltriethoxysilane and diisopropanolamine (DIPA) according to weight ratio 1:2~2.4
It is mixed, it is 118 ~ 124 DEG C that then heating, which keeps the temperature in reaction kettle, is stirred to react after 5 ~ 7h of processing and is filtered, subtracted
Pressure, distillation processing, it is spare to obtain mixture A after the completion；Using in the chlorine atom and diisopropanolamine (DIPA) in methyltriethoxysilane
Amino react, mixture A obtained is a kind of silane of modification；
B. it is passed through argon gas into reaction kettle, then will operate mixture A and absolute methanol, R- epoxychloropropane, second two made from a
Amine tetraacethyl disodium, sodium cellulosate, titanium dioxide are according to weight ratio 5 ~ 7:55~60:6~8:0.1~0.3：0.4~0.6:6 ~ 8 carry out
Mixing, it is 44 ~ 50 DEG C that then heating, which keeps the temperature in reaction kettle, and mixture B is taken out to obtain after being stirred to react 2.5 ~ 3.5h of processing
It is spare；Mixture A and R- epoxychloropropane ingredient occurs quaternization reaction and generates quaternary ammonium salt, later again in ethylenediamine tetra-acetic acid two
Under the action of sodium on the compound surface for grafting on titanium dioxide of sodium cellulosate, improve titanium dioxide surface group type and
Content, and chemical reaction ability, enhance chemisorption effect；
C. it is spare to obtain material C after mixture B made from operation b being carried out rotary evaporation, elution processing, is dried in vacuo；
D. material C and dispersant, deionized water obtained by c will be operated according to weight ratio 10 ~ 14:3~6:90 ~ 100 are mixed,
Then by step（3）Straw powder that treated is immersed in this solution, is filtered out straw powder after 1 ~ 2h of supersound process spare；
E. the straw powder obtained by operation d is put into spare after natural drying under room temperature；
（5）Carbonization treatment：
By step（4）Straw powder that treated, which is put into, carries out carbonization treatment in carbonizing apparatus, during which using nitrogen as environmental protection,
The temperature of control carbonization is 450 ~ 500 DEG C, is taken out after 1.5 ~ 2.5h of heat preservation carbonization treatment.It is carbonized again after modifying process
Processing, being fixed on the stable components of modification in biological carbon, and if carrying out modifying process after carbonization treatment again can influence
The quality of biological carbon own face causes whole using effect to reduce, bad stability.
Further, step（2）Described in quickly to unload to normal temperature and pressure be in completing to unload warm release processing in 2min.
Further, step（3）Described in citric acid solution in citric acid mass fraction be 10 ~ 15%.
Further, step（4）The grain diameter for operating the titanium dioxide described in b is 0.2 ~ 1 μm.
Further, step（4）The elution processing operated described in c is to carry out elution processing using anhydrous ether.
Further, step（4）It is low molecule wax class dispersant to operate the dispersant described in d.
Further, step（4）The supersonic frequency for operating the supersound process described in d is 180 ~ 220kHz.
The present invention provides a kind of special biological carbon preparation methods, have been made using agricultural crop straw a kind of best in quality
For repairs improvement soil environment biological carbon.Wherein, after first cleaning and crush stalk, then the steaming of high temperature and pressure is carried out to it
Vapour explosion treatment, the effective loose institutional framework of straw powder, improves fibre gap and specific surface area, is subsequent processing
It lays a good foundation, has then carried out citric acid solution immersion treatment, tissue space is further expanded using acid solution, promote thin
The further refinement of small fiber, improves specific surface area, has activated surface characteristic, has carried out modifying process later, to stalk fibre
The titanium dioxide granule ingredient secured by specially treated is penetrated into dimension, on the one hand can promote whole specific surface area, is increased
The strong adsorption capacity of subsequent bio carbon, on the other hand its a large amount of active group contained can enhance biological carbon to heavy metal etc.
The chemical bonding of harmful components is adsorbed, and the effect to soil remediation is improved；Finally carry out carbonization treatment, effectively by it is above-mentioned at
Divide and be stabilized in biological carbon, improves whole stability in use and quality.
The present invention has the following advantages compared with prior art：
The present invention provides a kind of preparation method of biological carbon, integrated artistic specification, process collocation is reasonable, biology obtained
The large specific surface area of carbon, adsorption capacity is strong, strong to the adsorption capacity of the harmful elements ingredients such as heavy metal in soil, can be significant
Promote safety of soil environment, great application value.
Specific implementation mode
Embodiment 1
A kind of preparation method of biological carbon for rehabilitating soil environment, includes the following steps：
（1）Stalk pretreatment：
Stalk cleaned up with clear water after drying, then put into pulverizer and crush processing, smashes it through 80 mesh
It is spare to obtain straw powder；
（2）High temperature high pressure process：
By step（1）The straw powder of gained is put into vapor tight tank, is passed through high-temperature vapor into vapor tight tank, while by vapor tight tank
Interior pressure increases to 0.5MPa, is quickly unloaded again to normal temperature and pressure, is finally taken out straw powder standby after heat-insulation pressure keeping processing 20min
With；
（3）Immersion treatment：
By step（2）Treated, and straw powder is immersed in citric acid solution, is taken out after immersion treatment 8min, is rushed with deionized water
It is spare after washing one time；
（4）Modifying process：
A. argon gas is passed through into reaction kettle, then by methyltriethoxysilane and diisopropanolamine (DIPA) according to weight ratio 1:2 carry out
Mixing, it is 118 DEG C that then heating, which keeps the temperature in reaction kettle, is stirred to react after handling 5h and is filtered, depressurized, at distillation
It is spare to obtain mixture A after the completion for reason；
B. it is passed through argon gas into reaction kettle, then will operate mixture A and absolute methanol, R- epoxychloropropane, second two made from a
Amine tetraacethyl disodium, sodium cellulosate, titanium dioxide are according to weight ratio 5:55:6:0.1：0.4:6 are mixed, and then heating is kept
Temperature in reaction kettle is 44 DEG C, be stirred to react after processing 2.5h take out mixture B is spare；
C. it is spare to obtain material C after mixture B made from operation b being carried out rotary evaporation, elution processing, is dried in vacuo；
D. material C and dispersant, deionized water obtained by c will be operated according to weight ratio 10:3:90 are mixed, then by step
（3）Straw powder that treated is immersed in this solution, is filtered out straw powder after supersound process 1h spare；
E. the straw powder obtained by operation d is put into spare after natural drying under room temperature；
（5）Carbonization treatment：
By step（4）Straw powder that treated, which is put into, carries out carbonization treatment in carbonizing apparatus, during which using nitrogen as environmental protection,
The temperature of control carbonization is 450 DEG C, is taken out after heat preservation carbonization treatment 1.5h.
Further, step（2）Described in quickly to unload to normal temperature and pressure be in completing to unload warm release processing in 2min.
Further, step（3）Described in citric acid solution in citric acid mass fraction be 10%.
Further, step（4）The grain diameter for operating the titanium dioxide described in b is 0.2 ~ 1 μm.
Further, step（4）The elution processing operated described in c is to carry out elution processing using anhydrous ether.
Further, step（4）It is low molecule wax class dispersant to operate the dispersant described in d.
Further, step（4）The supersonic frequency for operating the supersound process described in d is 180kHz.
Embodiment 2
A kind of preparation method of biological carbon for rehabilitating soil environment, includes the following steps：
（1）Stalk pretreatment：
Stalk cleaned up with clear water after drying, then put into pulverizer and crush processing, smashes it through 80 mesh
It is spare to obtain straw powder；
（2）High temperature high pressure process：
By step（1）The straw powder of gained is put into vapor tight tank, is passed through high-temperature vapor into vapor tight tank, while by vapor tight tank
Interior pressure increases to 0.53MPa, is quickly unloaded again to normal temperature and pressure, is finally taken out straw powder standby after heat-insulation pressure keeping processing 22min
With；
（3）Immersion treatment：
By step（2）Treated, and straw powder is immersed in citric acid solution, is taken out after immersion treatment 9min, is rushed with deionized water
It is spare after washing one time；
（4）Modifying process：
A. argon gas is passed through into reaction kettle, then by methyltriethoxysilane and diisopropanolamine (DIPA) according to weight ratio 1:2.2 into
It goes and mixes, it is 120 DEG C that then heating, which keeps the temperature in reaction kettle, is stirred to react after handling 6h and is filtered, depressurized, at distillation
It is spare to obtain mixture A after the completion for reason；
B. it is passed through argon gas into reaction kettle, then will operate mixture A and absolute methanol, R- epoxychloropropane, second two made from a
Amine tetraacethyl disodium, sodium cellulosate, titanium dioxide are according to weight ratio 6:58:7:0.2：0.5:7 are mixed, and then heating is kept
Temperature in reaction kettle is 46 DEG C, be stirred to react after processing 3h take out mixture B is spare；
C. it is spare to obtain material C after mixture B made from operation b being carried out rotary evaporation, elution processing, is dried in vacuo；
D. material C and dispersant, deionized water obtained by c will be operated according to weight ratio 12:5:96 are mixed, then by step
（3）Straw powder that treated is immersed in this solution, is filtered out straw powder after supersound process 1.5h spare；
E. the straw powder obtained by operation d is put into spare after natural drying under room temperature；
（5）Carbonization treatment：
By step（4）Straw powder that treated, which is put into, carries out carbonization treatment in carbonizing apparatus, during which using nitrogen as environmental protection,
The temperature of control carbonization is 480 DEG C, is taken out after heat preservation carbonization treatment 2h.
Further, step（2）Described in quickly to unload to normal temperature and pressure be in completing to unload warm release processing in 2min.
Further, step（3）Described in citric acid solution in citric acid mass fraction be 13%.
Further, step（4）The grain diameter for operating the titanium dioxide described in b is 0.2 ~ 1 μm.
Further, step（4）The elution processing operated described in c is to carry out elution processing using anhydrous ether.
Further, step（4）It is low molecule wax class dispersant to operate the dispersant described in d.
Further, step（4）The supersonic frequency for operating the supersound process described in d is 200kHz.
Embodiment 3
A kind of preparation method of biological carbon for rehabilitating soil environment, includes the following steps：
（1）Stalk pretreatment：
Stalk cleaned up with clear water after drying, then put into pulverizer and crush processing, smashes it through 80 mesh
It is spare to obtain straw powder；
（2）High temperature high pressure process：
By step（1）The straw powder of gained is put into vapor tight tank, is passed through high-temperature vapor into vapor tight tank, while by vapor tight tank
Interior pressure increases to 0.55MPa, is quickly unloaded again to normal temperature and pressure, is finally taken out straw powder standby after heat-insulation pressure keeping processing 24min
With；
（3）Immersion treatment：
By step（2）Treated, and straw powder is immersed in citric acid solution, is taken out after immersion treatment 10min, is used deionized water
It is spare after rinsing one time；
（4）Modifying process：
A. argon gas is passed through into reaction kettle, then by methyltriethoxysilane and diisopropanolamine (DIPA) according to weight ratio 1:2.4 into
It goes and mixes, it is 124 DEG C that then heating, which keeps the temperature in reaction kettle, is stirred to react after handling 7h and is filtered, depressurized, at distillation
It is spare to obtain mixture A after the completion for reason；
B. it is passed through argon gas into reaction kettle, then will operate mixture A and absolute methanol, R- epoxychloropropane, second two made from a
Amine tetraacethyl disodium, sodium cellulosate, titanium dioxide are according to weight ratio 7:60:8: 0.3：0.6:8 are mixed, and then heating is protected
It is 50 DEG C to hold temperature in reaction kettle, be stirred to react after processing 3.5h take out mixture B is spare；
C. it is spare to obtain material C after mixture B made from operation b being carried out rotary evaporation, elution processing, is dried in vacuo；
D. material C and dispersant, deionized water obtained by c will be operated according to weight ratio 14:6:100 are mixed, then will step
Suddenly（3）Straw powder that treated is immersed in this solution, is filtered out straw powder after supersound process 2h spare；
E. the straw powder obtained by operation d is put into spare after natural drying under room temperature；
（5）Carbonization treatment：
By step（4）Straw powder that treated, which is put into, carries out carbonization treatment in carbonizing apparatus, during which using nitrogen as environmental protection,
The temperature of control carbonization is 500 DEG C, is taken out after heat preservation carbonization treatment 2.5h.
Further, step（2）Described in quickly to unload to normal temperature and pressure be in completing to unload warm release processing in 2min.
Further, step（3）Described in citric acid solution in citric acid mass fraction be 15%.
Further, step（4）The grain diameter for operating the titanium dioxide described in b is 0.2 ~ 1 μm.
Further, step（4）The elution processing operated described in c is to carry out elution processing using anhydrous ether.
Further, step（4）It is low molecule wax class dispersant to operate the dispersant described in d.
Further, step（4）The supersonic frequency for operating the supersound process described in d is 220kHz.
Comparative example 1
This comparative example 1 compared with Example 2, eliminates step（4）Operation a, operation b in modifying process and operation c, and
With etc. mass parts commercially available titanium dioxide substitution operation d in material C ingredients, method and step all same in addition to this.
Comparative example 2
This comparative example 2 compared with Example 2, by step（4）Modifying process and step（5）The process of carbonization treatment carries out pair
It adjusts, that is, uses step（4）Processing method directly to biological carbon carry out modifying process, method and step all same in addition to this.
Control group
Existing conventional biological carbon preparation method.
In order to compare effect of the present invention, selects cotton stalk as experimental subjects, use above-described embodiment 2, comparison real respectively
It applies example 1, comparative example 2, the corresponding method of control group and is processed preparation biological carbon, then biological carbon is tested for the property
Experiment, specific correction data are as shown in table 1 below：
Table 1
Note：The corresponding index of each group, which is tested, in upper table 1 is specifically：Simulation soil remediation experiment is carried out, is weighed raw made from each group
Object carbon 0.05g, puts into the chromium solution of 30mL 55mg/L, adjusts pH=1, with 200 revs/min under conditions of temperature is 30 DEG C
The rotating speed of clock is stirred continuously, and measures the concentration of chromium in solution after 1h, 2h respectively, and is converted into the removal rate of chromium, corresponding to be exactly
1h chromium removal rate in These parameters and 2h chromium removal rates；Chromium content in solution is measured at regular intervals, and is converted into chromium
Removal rate, removal rate peak are the chromium total removal rate in These parameters；Then this solution again（Biological carbon is not filtered out）It puts
Enter to temperature be 45 DEG C under conditions of ultrasonic vibration handle 2h, measure chromium content in solution again, and be converted into the removal rate of chromium,
It is compared to the chromium rebound release rate that the percentage that chromium total removal rate declines is in These parameters.
The biological carbon made from the method for the present invention it can be seen from upper table 1 fixes energy for the absorption of harmful components in soil
Power is strong, and the quality of reparation is good, stability is high, the great market competitiveness and application value.
Claims (7)
1. a kind of preparation method of biological carbon for rehabilitating soil environment, which is characterized in that include the following steps：
（1）Stalk pretreatment：
Stalk cleaned up with clear water after drying, then put into pulverizer and crush processing, smashes it through 80 mesh
It is spare to obtain straw powder；
（2）High temperature high pressure process：
By step（1）The straw powder of gained is put into vapor tight tank, is passed through high-temperature vapor into vapor tight tank, while by vapor tight tank
Interior pressure increases to 0.5 ~ 0.55MPa, and heat-insulation pressure keeping is quickly unloaded again after handling 20 ~ 24min to normal temperature and pressure, finally by straw powder
It takes out spare；
（3）Immersion treatment：
By step（2）Treated, and straw powder is immersed in citric acid solution, is taken out after 8 ~ 10min of immersion treatment, is used deionization
Water is spare after rinsing one time；
（4）Modifying process：
A. argon gas is passed through into reaction kettle, then by methyltriethoxysilane and diisopropanolamine (DIPA) according to weight ratio 1:2~2.4
It is mixed, it is 118 ~ 124 DEG C that then heating, which keeps the temperature in reaction kettle, is stirred to react after 5 ~ 7h of processing and is filtered, subtracted
Pressure, distillation processing, it is spare to obtain mixture A after the completion；
B. it is passed through argon gas into reaction kettle, then will operate mixture A and absolute methanol, R- epoxychloropropane, second two made from a
Amine tetraacethyl disodium, sodium cellulosate, titanium dioxide are according to weight ratio 5 ~ 7:55~60:6~8:0.1~0.3：0.4~0.6:6 ~ 8 carry out
Mixing, it is 44 ~ 50 DEG C that then heating, which keeps the temperature in reaction kettle, and mixture B is taken out to obtain after being stirred to react 2.5 ~ 3.5h of processing
It is spare；
C. it is spare to obtain material C after mixture B made from operation b being carried out rotary evaporation, elution processing, is dried in vacuo；
D. material C and dispersant, deionized water obtained by c will be operated according to weight ratio 10 ~ 14:3~6:90 ~ 100 are mixed,
Then by step（3）Straw powder that treated is immersed in this solution, is filtered out straw powder after 1 ~ 2h of supersound process spare；
E. the straw powder obtained by operation d is put into spare after natural drying under room temperature；
（5）Carbonization treatment：
By step（4）Straw powder that treated, which is put into, carries out carbonization treatment in carbonizing apparatus, during which using nitrogen as environmental protection,
The temperature of control carbonization is 450 ~ 500 DEG C, is taken out after 1.5 ~ 2.5h of heat preservation carbonization treatment.
2. a kind of preparation method of biological carbon for rehabilitating soil environment according to claim 1, which is characterized in that step
Suddenly（2）Described in quickly to unload to normal temperature and pressure be in completing to unload warm release processing in 2min.
3. a kind of preparation method of biological carbon for rehabilitating soil environment according to claim 1, which is characterized in that step
Suddenly（3）Described in citric acid solution in citric acid mass fraction be 10 ~ 15%.
4. a kind of preparation method of biological carbon for rehabilitating soil environment according to claim 1, which is characterized in that step
Suddenly（4）The grain diameter for operating the titanium dioxide described in b is 0.2 ~ 1 μm.
5. a kind of preparation method of biological carbon for rehabilitating soil environment according to claim 1, which is characterized in that step
Suddenly（4）The elution processing operated described in c is to carry out elution processing using anhydrous ether.
6. a kind of preparation method of biological carbon for rehabilitating soil environment according to claim 1, which is characterized in that step
Suddenly（4）It is low molecule wax class dispersant to operate the dispersant described in d.
7. a kind of preparation method of biological carbon for rehabilitating soil environment according to claim 1, which is characterized in that step
Suddenly（4）The supersonic frequency for operating the supersound process described in d is 180 ~ 220kHz.
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| CN111659351A (en) * | 2020-07-14 | 2020-09-15 | 清华大学深圳国际研究生院 | Modified biological carbon capable of simultaneously releasing silicon and adsorbing heavy metals efficiently and preparation method thereof |
| CN113181877A (en) * | 2021-05-13 | 2021-07-30 | 沈阳农业大学 | Preparation method of magnetic biochar material |
| CN113429977A (en) * | 2021-06-25 | 2021-09-24 | 阳煤丰喜肥业（集团）有限责任公司闻喜复肥分公司 | Saline-alkali soil conditioner |
| CN114031457A (en) * | 2021-11-12 | 2022-02-11 | 绥化学院 | Long-acting slow-release compound fertilizer and preparation method thereof |
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