CN103949212A - Preparation method of biomass-based magnetic biochar - Google Patents
Preparation method of biomass-based magnetic biochar Download PDFInfo
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- CN103949212A CN103949212A CN201410145644.XA CN201410145644A CN103949212A CN 103949212 A CN103949212 A CN 103949212A CN 201410145644 A CN201410145644 A CN 201410145644A CN 103949212 A CN103949212 A CN 103949212A
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Abstract
The invention relates to a preparation method of biomass-based magnetic biochar. According to the preparation method, forestry and agricultural waste materials are taken as raw materials; biochar prepared via oxygen-limited pyrolysis or hydrothermal carbonization is taken as a substrate; magnetic nano-material Fe3O4 is obtained via iron precursor pyrolysis, loading of magnetic nano-material Fe3O4 onto the biochar substrate is realized in a polyhydric alcohol solution, and an obtained product is subjected to sintering under nitrogen protection so as to obtain stable magnetic nano particles with high crystallinity. Compared with existing technology, loading of in-situ synthesized Fe3O4 onto the surface of biochar is realized via pyrolysis; reaction selectivity and efficiency are high; size of the Fe3O4 nano particles and loading area on the surface of biochar are controllable; and operation is simple and convenient.
Description
Technical field
The invention belongs to agriculture and forestry organic waste material secondary resource and utilize technical field, be specifically related to a kind of preparation method of charcoal, especially relate to a kind of preparation method of biomass-based magnetic bio charcoal.
Background technology
Charcoal is the living beings rich carbon solids that low temperature pyrolyzer produces under limited oxygen condition, and its raw material sources are extensive, comprise many agriculture and forestry organic waste materials such as rice husk, camphor tree branch, bamboo, animal dung matter.Different from other carbonated material (as active carbon), charcoal is mainly used as soil additive to promote soil fertility and to increase soil carbon sink, and it can affect Transport And Transformation behavior and the biological effectiveness of the hazardous contaminant such as heavy metal and organic pollution.But charcoal is often difficult to separate recovery after Adsorption pollutant, easily causes the wasting of resources and secondary pollution, and the introducing of magnetic nanoparticle separating bio charcoal fast.
The magnetic Carbon Materials of preparation at present, as magnetic active carbon, magnetic multi-walled carbon nano-tubes etc., mostly by chemical precipitation method or infusion process, above-mentioned magnetic nanoparticle are deposited on to living beings surface and make by the charing of limit oxygen, but magnetic medium are generally γ-Fe
2o
3magnetic is strong not.
Summary of the invention
Object of the present invention is exactly that to provide one to be intended to solve prior art preparation process in order to overcome the defect that above-mentioned prior art exists loaded down with trivial details, the preparation method of the biomass-based magnetic bio charcoal of long defect of production cycle.
Object of the present invention can be achieved through the following technical solutions:
A preparation method for biomass-based magnetic bio charcoal, is characterized in that, the method is that charcoal is mixed with the alcoholic solution of iron content precursor, and iron content precursor pyrolytic makes magnetic nanoparticle and is carried on charcoal, obtains product.
Described method specifically comprises the following steps:
(1) charcoal is sieved 30～120 orders, obtain the biological particles of different-grain diameter;
(2) pickling biological particles, removes surface impurity;
(3) step (2) biological particles after treatment is joined in polyhydric alcohol solutions, ultrasonic 5min, again iron precursor is joined in above-mentioned solution, iron precursor and biological particles mass ratio are 2: 1, ultrasonic 10min is heated to 180 DEG C of reaction 0.5h under the state of the logical nitrogen of magnetic agitation, continues to be heated to 270～280 DEG C, reaction 0.5～1h, makes magnetic bio charcoal;
(4) magnetic bio charcoal step (3) being made is cooled to room temperature, and cleans, is dried;
(5) dried magnetic bio charcoal is placed in to 100～500 DEG C of nitrogen protection atmosphere and carries out sintering.Sintering can obtain certain crystalline form, crystallite granularity, aperture and specific area, and the mechanical strength of magnetic bio charcoal is larger.
Described charcoal is taking agriculture and forestry organic waste material as raw material is directly taking agriculture and forestry organic waste material as raw material, makes through limit oxygen pyrolysis or hydro-thermal charing method; Described agriculture and forestry organic waste material is one or more in rice husk, camphor tree branch, bamboo or cow dung.
The surface area of described charcoal is 50.35～130.34m
2/ g, pore volume is 0.0592～0.1522cm
3/ g, described magnetic nanoparticle size and coverage density are controlled by the following method: change the concentration of iron precursor and the mass ratio of iron precursor and charcoal.Magnetic nanoparticle is good dispersion in water.
Magnetic nanoparticle is in polyalcohol system, to carry out pyrolytic gained taking Organic Iron as precursor, and the nanoparticle size making is little.
Described iron precursor is ferric acetyl acetonade or carbonyl iron.
Described polyalcohol is one or more in ethylene glycol, diethylene glycol, triethylene glycol or TEG.
Magnetic bio Carbon Materials prepared by the present invention is directly taking agriculture and forestry organic waste material (as rice husk, camphor tree branch, bamboo etc.) as raw material, in polyhydric alcohol solutions, by the magnetic Nano material Fe of iron precursor pyrolytic one-tenth
3o
4be carried on charcoal, then under nitrogen protection, carry out sintering, magnetic nanoparticle degree of crystallinity is high and stable.
Compared with prior art, the present invention has following characteristics:
1. the present invention is taking agriculture and forestry organic waste material as raw material, and preparation method is simple, with low cost;
2. the magnetic bio charcoal that the present invention makes easily decomposes in the aqueous solution, as adsorbent, because it has also easy centralized recovery recycling of ferromagnetism;
3. the present invention has realized the synthetic Fe of original position by the method for pyrolytic
3o
4nano material is carried on charcoal surface, and reaction selectivity is strong, and efficiency is high, Fe
3o
4size, crystal formation, crystallite granularity, aperture, specific area and the load area on charcoal surface of nano particle are all controlled.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1
By the charcoal of preparation 30 orders that sieve, pickling; Take 1g charcoal and be placed in 300mL ethylene glycol solution, ultrasonic 5min; And then add 2g ferric acetyl acetonade (Fe (acac)
3), under the state of the logical nitrogen of magnetic agitation, be heated to 180 DEG C of reaction 0.5h, continue to be heated to 275 DEG C of reaction 0.5h, cooling, cleaning, dry, then sintering under 100 DEG C of nitrogen protections.
Embodiment 2
By the charcoal of preparation 60 orders that sieve, pickling; Take 1g charcoal and be placed in 150mL ethylene glycol solution, ultrasonic 5min; And then add 2g ferric acetyl acetonade Fe (acac)
3, under the state of the logical nitrogen of magnetic agitation, be heated to 180 DEG C of reaction 0.5h, continue to be heated to 275 DEG C of reaction 0.5h, cooling, cleaning, dry, then sintering under 200 DEG C of nitrogen protections.
Embodiment 3
By the charcoal of preparation 90 orders that sieve, pickling; Take 1g charcoal and be placed in 100mL ethylene glycol solution, ultrasonic 5min; And then add 2g ferric acetyl acetonade Fe (acac)
3, under the state of the logical nitrogen of magnetic agitation, be heated to 180 DEG C of reaction 0.5h, continue to be heated to 275 DEG C of reaction 0.5h, cooling, cleaning, dry, then sintering under 300 DEG C of nitrogen protections.
Embodiment 4
By the charcoal of preparation 120 orders that sieve, pickling; Take 1g charcoal and be placed in 100mL diethylene glycol solution, ultrasonic 5min; And then add 2g ferric acetyl acetonade Fe (acac)
3, under the state of the logical nitrogen of magnetic agitation, be heated to 180 DEG C of reaction 0.5h, continue to be heated to 275 DEG C of reaction 0.5h, cooling, cleaning, dry, then sintering under 400 DEG C of nitrogen protections.
Embodiment 6
By the charcoal of preparation 120 orders that sieve, pickling; Take 1g charcoal and be placed in 100mL triethylene glycol solution, ultrasonic 5min; And then add 2g ferric acetyl acetonade Fe (acac)
3, under the state of the logical nitrogen of magnetic agitation, be heated to 180 DEG C of reaction 0.5h, continue to be heated to 275 DEG C of reaction 1h, cooling, cleaning, dry, then sintering under 500 DEG C of nitrogen protections.
Embodiment 7
By the charcoal of preparation 120 orders that sieve, pickling; Take 1g charcoal and be placed in 100mL TEG solution, ultrasonic 5min; And then add 2g ferric acetyl acetonade Fe (acac)
3, under the state of the logical nitrogen of magnetic agitation, be heated to 180 DEG C of reaction 0.5h, continue to be heated to 275 DEG C of reaction 1h, cooling, cleaning, dry, then sintering under 300 DEG C of nitrogen protections.
Embodiment 8
By the charcoal of preparation 120 orders that sieve, pickling; Take 1g charcoal and be placed in 100mL triethylene glycol solution, ultrasonic 5min; And then add 2g carbonyl iron Fe (CO)
5, under the state of the logical nitrogen of magnetic agitation, be heated to 180 DEG C of reaction 0.5h, continue to be heated to 275 DEG C of reaction 1h, cooling, cleaning, dry, then sintering under 300 DEG C of nitrogen protections.
Embodiment 9
A preparation method for biomass-based magnetic bio charcoal, the method is that charcoal is mixed with the alcoholic solution of iron content precursor, iron content precursor pyrolytic makes magnetic nanoparticle and is carried on charcoal, obtains product.
Described method specifically comprises the following steps:
(1) taking agriculture and forestry organic waste material as raw material is directly taking agriculture and forestry organic waste material as raw material, make charcoal through limit oxygen pyrolysis or hydro-thermal charing method, the surface area of gained charcoal is 50.35m
2/ g, pore volume is 0.0592cm
3/ g, by charcoal 30～120 orders that sieve, obtains the biological particles of different-grain diameter; Described agriculture and forestry organic waste material is one or more in rice husk, camphor tree branch, bamboo or cow dung.
(2) pickling biological particles, removes surface impurity;
(3) step (2) biological particles after treatment is joined in ethylene glycol solution, ultrasonic 5min, again iron precursor ferric acetyl acetonade is joined in above-mentioned solution, iron precursor and biological particles mass ratio are 2: 1, ultrasonic 10min is heated to 180 DEG C of reaction 0.5h under the state of the logical nitrogen of magnetic agitation, continues to be heated to 270 DEG C, reaction 1h, makes magnetic bio charcoal; Be magnetic nanoparticle, change the concentration of iron precursor and the mass ratio of iron precursor and charcoal, can control magnetic nanoparticle size and coverage density;
(4) magnetic bio charcoal step (3) being made is cooled to room temperature, and cleans, is dried;
(5) dried magnetic bio charcoal is placed in to 100 DEG C of nitrogen protection atmosphere and carries out sintering.Sintering can obtain certain crystalline form, crystallite granularity, aperture and specific area, and the mechanical strength of magnetic bio charcoal is larger.
Embodiment 10
A preparation method for biomass-based magnetic bio charcoal, the method is that charcoal is mixed with the alcoholic solution of iron content precursor, iron content precursor pyrolytic makes magnetic nanoparticle and is carried on charcoal, obtains product.
Described method specifically comprises the following steps:
(1) taking agriculture and forestry organic waste material as raw material is directly taking agriculture and forestry organic waste material as raw material, make charcoal through limit oxygen pyrolysis or hydro-thermal charing method, the surface area of gained charcoal is 130.34m
2/ g, pore volume is 0.1522cm
3/ g, by charcoal 30～120 orders that sieve, obtains the biological particles of different-grain diameter; Described agriculture and forestry organic waste material is one or more in rice husk, camphor tree branch, bamboo or cow dung.
(2) pickling biological particles, removes surface impurity;
(3) step (2) biological particles after treatment is joined in triethylene glycol solution, ultrasonic 5min, again iron precursor carbonyl iron is joined in above-mentioned solution, iron precursor and biological particles mass ratio are 2: 1, ultrasonic 10min is heated to 180 DEG C of reaction 0.5h under the state of the logical nitrogen of magnetic agitation, continues to be heated to 280 DEG C, reaction 0.5h, makes magnetic bio charcoal; Be magnetic nanoparticle, change the concentration of iron precursor and the mass ratio of iron precursor and charcoal, can control magnetic nanoparticle size and coverage density;
(4) magnetic bio charcoal step (3) being made is cooled to room temperature, and cleans, is dried;
(5) dried magnetic bio charcoal is placed in to 500 DEG C of nitrogen protection atmosphere and carries out sintering.Sintering can obtain certain crystalline form, crystallite granularity, aperture and specific area, and the mechanical strength of magnetic bio charcoal is larger.
Claims (6)
1. a preparation method for biomass-based magnetic bio charcoal, is characterized in that, the method is that charcoal is mixed with the alcoholic solution of iron content precursor, and iron content precursor pyrolytic makes magnetic nanoparticle and is carried on charcoal, obtains product.
2. the preparation method of a kind of biomass-based magnetic bio charcoal according to claim 1, is characterized in that, described method specifically comprises the following steps:
(1) charcoal is sieved 30～120 orders, obtain the biological particles of different-grain diameter;
(2) pickling biological particles, removes surface impurity;
(3) step (2) biological particles after treatment is joined in polyhydric alcohol solutions, ultrasonic 5min, again iron precursor is joined in above-mentioned solution, iron precursor and biological particles mass ratio are 2: 1, ultrasonic 10min is heated to 180 DEG C of reaction 0.5h under the state of the logical nitrogen of magnetic agitation, continues to be heated to 270～280 DEG C, reaction 0.5～1h, makes magnetic bio charcoal;
(4) magnetic bio charcoal step (3) being made is cooled to room temperature, and cleans, is dried;
(5) dried magnetic bio charcoal is placed in to 100～500 DEG C of nitrogen protection atmosphere and carries out sintering.
3. the preparation method of a kind of biomass-based magnetic bio charcoal according to claim 1 and 2, is characterized in that, described charcoal is taking agriculture and forestry organic waste material as raw material is directly taking agriculture and forestry organic waste material as raw material, makes through limit oxygen pyrolysis or hydro-thermal charing method; Described agriculture and forestry organic waste material is one or more in rice husk, camphor tree branch, bamboo or cow dung.
4. the preparation method of a kind of biomass-based magnetic bio charcoal according to claim 1 and 2, is characterized in that, the surface area of described charcoal is 50.35～130.34m
2/ g, pore volume is 0.0592～0.1522cm
3/ g, described magnetic nanoparticle size and coverage density are controlled by the following method: change the concentration of iron precursor and the mass ratio of iron precursor and charcoal.
5. the preparation method of a kind of biomass-based magnetic bio charcoal according to claim 1, is characterized in that, described iron precursor is ferric acetyl acetonade or carbonyl iron.
6. the preparation method of a kind of biomass-based magnetic bio charcoal according to claim 1, is characterized in that, described polyalcohol is one or more in ethylene glycol, diethylene glycol, triethylene glycol or TEG.
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| CN104432538A (en) * | 2014-11-07 | 2015-03-25 | 中国烟草总公司郑州烟草研究院 | Preparation method for charcoal heat supply body for heating non-combustion-type tobacco products |
| CN104549155A (en) * | 2015-01-23 | 2015-04-29 | 中国科学院生态环境研究中心 | Biological activated carbon composite material and application thereof |
| CN105396551A (en) * | 2015-12-15 | 2016-03-16 | 浙江工业大学 | Iron-containing biochar prepared from rice roots and application thereof in adsorption and solidification of heavy metal ions |
| CN105712496A (en) * | 2016-04-19 | 2016-06-29 | 肥东县柯文斌家庭农场 | Water body clarifying agent for removing eutrophication substances |
| CN105712495A (en) * | 2016-04-19 | 2016-06-29 | 肥东县柯文斌家庭农场 | Water body clarifying agent capable of improving water body self-purifying capacity |
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| CN105797681A (en) * | 2016-04-15 | 2016-07-27 | 江西农业大学 | Preparing method for micron/nano water-dispersible biochar |
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