CN103406095A - Activation method and application of biomass liquefaction residue - Google Patents
Activation method and application of biomass liquefaction residue Download PDFInfo
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- CN103406095A CN103406095A CN2013102967363A CN201310296736A CN103406095A CN 103406095 A CN103406095 A CN 103406095A CN 2013102967363 A CN2013102967363 A CN 2013102967363A CN 201310296736 A CN201310296736 A CN 201310296736A CN 103406095 A CN103406095 A CN 103406095A
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Abstract
The invention belongs to the technical fields of environmental protection and comprehensive utilization of resources, and particularly relates to a biomass liquefaction residue activation method for recycling a biomass hydrothermal liquefaction residue and application of the biomass liquefaction residue. The specific process comprises the following steps: (1) activating a biomass liquefaction residue with acid or alkali to generate activated carbon particles; (2) performing in-situ synthesis on the activated carbon particles to generate magnetic particles, wherein the magnetic carbon material has high specific surface area, high pore volume and high magnetic intensity, and can be magnetically separated from a water solution; and (3) removing organic dye pollutants in wastewater with the magnetic carbon material. The invention has important promotion action on development of the biomass industry. The preparation method has the advantages of low energy consumption, environment friendliness, mild conditions, simple process, high adsorption capacity for dye organic pollutants, no secondary pollution and the like.
Description
Technical field
The invention belongs to environmental protection and comprehensive utilization of resources technical field, be specifically related to biomass by hydro-thermal liquefied residue recycling, for a kind of with biomass liquefying residue activation method and uses thereof.
Background technology
At present, the large scale mining utilization of fossil energy and the existence of the problems such as the environmental pollution caused and global warming thereof, make the living beings utilization in energy consumption structure, occupy more and more consequence.China's biomass resource is abundant, and a large amount of going out of use or burning, and causes serious environmental pollution.The hydro-thermal liquefaction of living beings can be translated into liquid bio oil and solid-state biological carbon materials, and this is a kind of high effective way that living beings are utilized.The Carbon Materials that biomass liquefying obtains has the nucleocapsid structure character of armaticity, and possesses certain activity; But its specific area is low, cause it to organic pollutions such as dyestuffs, almost there is no adsorption effect; In addition, it also has and is difficult to separate to reclaim shortcoming, easily causes the wasting of resources and secondary pollution.Therefore, biological carbon materials can not directly be used for wastewater treatment as sorbing material.
By the biological carbon materials chemical activation, can prepare and have porous character and the high active carbon of specific area; Again magnetic medium is introduced to active carbon, be expected to prepare and a kind ofly can effectively adsorb organic dye pollutant, can realize the novel magnetic charcoal sorbing material that it effectively separates by magnetic separation technique again.
The present invention be take the biomass by hydro-thermal liquefied residue and is raw material, by activation with compose magnetization two steps, prepare novel high-ratio surface and the magnetic Carbon Materials of high pore volume, can effectively remove the organic dye pollutant in environment, and can realize the magnetic separation.For abandoned biomass hydro-thermal liquefied residue has found an effective disposal technology.
Summary of the invention
The invention provides a kind of preparation method and its usage of biomass by hydro-thermal liquefied residue material as the magnetic Carbon Materials of raw material of take.
Preparation method's concrete technology of magnetic bio Carbon Materials comprises the steps:
(1) the biomass by hydro-thermal liquefied residue is added in the acid of 10%-60% or 100-300g/L salt activator solution and soaks 2-48 hour, dry, wherein acid or salt activator are preferably the alkaline metal salts such as inorganic acid and alkali metal chloride, alkali metal hydroxide, alkali carbonate, and wherein the mass ratio of biological carbon materials and acid or salt is preferably 1:1-1:6.
(2) biological carbon materials after step (1) oven dry is put into to porcelain week, be placed in high temperature box furnace, under the nitrogen atmosphere protection, rise to 400-800 ℃, and maintain 30-240min.After temperature is cooled to room temperature, take out, washing, drying, get final product to obtain activated carbon granule.
(3) step (3) gained activated carbon granule is added in iron salt solutions, and the mass ratio of active carbon and ferriferous oxide is preferably 1:1-1:4,40-100 ℃ of water-bath, stirs the lower alkaline solution that drips certain mass concentration, and ageing 1-6 hour.Solid material after filtration, after washing and drying, obtain the magnetic Carbon Materials.Wherein, alkaline solution is that concentration is the 1-6mol/L alkali hydroxide soln, and iron salt solutions is the mixed solution of divalent iron salt and trivalent iron salt, and molar concentration is preferably 10-60 mmol/L, and mol ratio is preferably 1:1-1:4.
(4) the magnetic Carbon Materials of gained has magnetic preferably, by externally-applied magnetic field, can well, from solution, removing, avoid secondary pollution and the wasting of resources.
(5) the magnetic Carbon Materials of gained is for removing the organic dye pollutant of waste water.The concentration that adds of magnetic Carbon Materials is preferably 200-1000mg/L.
(6) preparation flow of the present invention is simple, with low cost; Iron form on the magnetic Carbon Materials particle made is mainly Fe
3O
4, γ-Fe
2O
3And FeOOH, Stability Analysis of Structures, be easy to magnetic and separate.
The accompanying drawing explanation
Fig. 1: preparation method's flow chart of the present invention.
Fig. 2: the absorption isotherm of product to the malachite green dyestuff.
The specific embodiment
The following examples, for further illustrating the present invention, are not limitation of the invention.
Embodiment 1
(1) dry salix monogolica biomass by hydro-thermal liquefied residue, 20 orders sieve; The residue that will sieve is added to K
2CO
3In the aqueous solution, soaked 24 hours, dry, wherein material and K
2CO
3Mass ratio be 1:2.Biological carbon materials after drying is put into to porcelain week, put in high temperature box furnace, the heating rate with 4 ℃/min under the nitrogen atmosphere protection rises to 700 ℃, and maintains 90min.After temperature is cooled to room temperature, take out, washing, drying, get final product to obtain activated carbon granule AC-1.Through specific surface area measuring instrument, measure, its specific area is 1230m
2/ g, the pore volume of total hole and micropore are 0.81 and 0.55cm
3g
-1.
Embodiment 2
(2) drying of rice straw biologic matter hydro-thermal liquefied residue, 20 orders sieve; The residue that will sieve is added to K
2CO
3In the aqueous solution, soaked 24 hours, dry, wherein material and K
2CO
3Mass ratio be 1:2.Biological carbon materials after drying is put into to porcelain week, put in high temperature box furnace, the heating rate with 4 ℃/min under the nitrogen atmosphere protection rises to 700 ℃, and maintains 90min.After temperature is cooled to room temperature, take out, washing, drying, get final product to obtain activated carbon granule AC-2.Through specific surface area measuring instrument, measure, its specific area is 1334m
2/ g, the pore volume of total hole and micropore are 1.07 and 0.50cm
3g
-1.
Embodiment 3
Activated carbon granule AC-1,20 orders that sieve, be added in iron salt solutions, and active carbon and mass ratio ferriferous oxide are 1:1, and iron salt solutions is FeCl
3And FeSO
4 .7H
2The mixed solution of O, mol ratio is preferably 1:1.Under 70 ℃ of water-baths, the 5mol/LNaOH solution of agitation and dropping 100mL, and ageing 3 hours.After solid material filtration, washing and drying, obtain magnetic Carbon Materials M-1.Through specific surface area measuring instrument, measure, its specific area is 673m
2/ g, the pore volume of total hole and micropore are 0.65 and 0.28cm
3g
-1.The magnetic Carbon Materials made is measured through the vibrating specimen magnetometer analyzer, and saturated magnetic intensity is 38.5emu/g.
Embodiment 4
Activated carbon granule AC-2,20 orders that sieve, be added in iron salt solutions, and active carbon and mass ratio ferriferous oxide are 1:1, and iron salt solutions is FeCl
3And FeSO
4 .7H
2The mixed solution of O, mol ratio is preferably 1:1.Under 70 ℃ of water-baths, the 5mol/LNaOH solution of agitation and dropping 100mL, and ageing 3 hours.After solid material filtration, washing and drying, obtain magnetic Carbon Materials M-2.Through specific surface area measuring instrument, measure, its specific area is 674m
2/ g, the pore volume of total hole and micropore are 0.72 and 0.24cm
3g
-1.The magnetic Carbon Materials made is measured through the vibrating specimen magnetometer analyzer, and saturated magnetic intensity is 12.4emu/g.
Embodiment 5
Material M-1,0.04g join 80mL malachite green concentration and are respectively 62.5,125,187.5,250,375 and the solution of 500ppm in, be placed in the isothermal vibration case, under 25 ℃ and 200rpm, shake 24h.Get the 5mL supernatant, filter, on ultraviolet specrophotometer, measure the concentration of residue malachite green.As calculated, the magnetic Carbon Materials made is 486mgg to the maximum saturation adsorption capacity of malachite green
-1.
Embodiment 6
Material M-2,0.04g join 80mL malachite green concentration and are respectively 62.5,125,187.5,250,375 and the solution of 500ppm in, be placed in the isothermal vibration case, under 25 ℃ and 200rpm, shake 24h.Get the 5mL supernatant, filter, on ultraviolet specrophotometer, measure the concentration of residue malachite green.As calculated, the magnetic Carbon Materials made is 625mgg to the maximum saturation adsorption capacity of malachite green
-1.
Fig. 2 is the magnetic Carbon Materials M-1 that makes and the M-2 adsorption capacity figure to malachite green, and as seen from the figure, along with the increase of equilibrium concentration, the adsorption capacity of magnetic Carbon Materials increases gradually, finally tends towards stability.
Embodiment 7
It is that in the solution of 250ppm, pH is respectively 3,4 that material M-1,0.04g join 80mL malachite green concentration, 5,6,7,8 and 9.Be placed in the isothermal vibration case, shake 24h under 25 ℃ and 200rpm.Get the 5mL supernatant, filter, on ultraviolet specrophotometer, measure the concentration of residue malachite green.As calculated, be respectively 3,4 in initial soln pH value, under 5,6,7,8 and 9 conditions, the magnetic Carbon Materials made is respectively 85.5%, 87.3% to the removal efficiency of malachite green, and 87.5%, 86.6%, 86.6%, 91.6% and 94.2%.Under condition of different pH, the magnetic Carbon Materials made all can be removed the solution Malachite Green preferably.
Claims (6)
1. the activation method of a biomass liquefying residue is characterized in that the method realizes by following concrete steps:
The biomass by hydro-thermal liquefied residue is added in the acid of 10 %-60 % or 100-300g/L salt activator solution and soaks 2-48 hour, dry;
Biological carbon materials after oven dry is put into porcelain week, is placed in high temperature box furnace, and pyrolysis under the nitrogen atmosphere protection, after temperature is cooled to room temperature, take out, washing, and drying, get final product to obtain activated carbon granule;
Activated carbon granule is added in iron salt solutions, at 40-100 ℃ of temperature, drips the alkaline solution of certain mass concentration, and ageing, solid material after filtration, after washing and drying, obtain the magnetic Carbon Materials;
Wherein,
The mass ratio of hydro-thermal liquefied residue and acid or salt is 1:1-1:6, pyrolysis temperature 400-800 ℃, and maintain 30-240 min;
Alkaline solution is that concentration is the 1-6mol/L alkali hydroxide soln;
The mass ratio of active carbon and ferriferous oxide is 1:1-1:4, and iron salt solutions is the mixed solution of divalent iron salt and trivalent iron salt, and molar concentration is 10-60 mmol/L, and mol ratio is 1:1-1:4;
The ageing condition is 1-6 hour under 40-100 ℃ of water-bath.
2. according to claim 1ly a kind ofly take the biomass liquefying residue as raw material prepares the preparation method of magnetic Carbon Materials, it is characterized in that described biomass by hydro-thermal liquefied residue is the living beings such as agricultural stalk, trees, algae generate under the hydro-thermal liquefaction condition liquefied residue.
3. according to claim 1ly a kind ofly take the biomass liquefying residue as raw material prepares the preparation method of magnetic Carbon Materials, it is characterized in that biological carbon materials and acid or salt activator comprise the alkaline metal salts such as inorganic acid and alkali metal chloride, alkali metal hydroxide, alkali carbonate.
4. according to claim 1ly a kind ofly take the biomass liquefying residue as raw material prepares the preparation method of magnetic Carbon Materials, it is characterized in that alkaline solution is that concentration is 1-6 mol/L alkali hydroxide soln.
5. take the biomass liquefying residue as raw material prepares the purposes of magnetic Carbon Materials for one kind, it is characterized in that: the magnetic Carbon Materials is for removing the organic dye pollutant of waste water.
6. a kind ofly according to claim 5 take the biomass liquefying residue as raw material prepares the purposes of magnetic Carbon Materials, it is characterized in that the concentration that adds of magnetic Carbon Materials is 200-1000 mg/L.
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|---|---|---|---|---|
| CN103657602A (en) * | 2013-12-03 | 2014-03-26 | 湖南大学 | Biological adsorbent, preparation method thereof, and application thereof to removal of methylene blue dye of waste water |
| CN104492382A (en) * | 2013-12-06 | 2015-04-08 | 东华理工大学 | Preparation method of carboxylation hydrothermal biomass charcoal for remedying uranium-containing wastewater |
| CN105126755A (en) * | 2015-09-10 | 2015-12-09 | 哈尔滨工业大学宜兴环保研究院 | Novel magnetic active carbon and preparation method thereof |
| CN105439238A (en) * | 2015-12-11 | 2016-03-30 | 哈尔滨工业大学宜兴环保研究院 | Method for integrated treatment of dyeing wastewater by using magnetic activated carbon |
| CN105731452A (en) * | 2016-01-22 | 2016-07-06 | 青岛大学 | Active carbon electrode material as well as preparation method and application thereof |
| CN105753608A (en) * | 2016-05-17 | 2016-07-13 | 北京化工大学 | Preparation method and application of novel iron-based biochar |
| CN107029535A (en) * | 2017-03-01 | 2017-08-11 | 沃邦环保有限公司 | A kind of deodorant compositions and its application for being used to cultivate night soil-treatment |
| CN107096500A (en) * | 2017-05-02 | 2017-08-29 | 中国药科大学 | A kind of utilization Chinese medicine slag prepares the method for magnetic bio charcoal, magnetic bio charcoal and application |
| CN108745288A (en) * | 2018-06-23 | 2018-11-06 | 铜仁学院 | A kind of magnetism oil tea shell biomass carbon and preparation method thereof |
| CN108940204A (en) * | 2018-08-14 | 2018-12-07 | 河南工业大学 | The preparation method of the magnetic cow dung base charcoal of perchlorate in Adsorption water |
| CN110467945A (en) * | 2019-06-27 | 2019-11-19 | 江苏大学 | A kind of method that the voluminous object of microalgae liquefaction participates in the copyrolysis upgrading of kitchen abandoned oil |
| CN111484191A (en) * | 2020-03-24 | 2020-08-04 | 江苏大学 | Sewage enhanced treatment method based on microalgae and hydrothermal liquefied biochar thereof |
| CN112642407A (en) * | 2020-12-14 | 2021-04-13 | 北京林业大学 | Method for preparing adsorption material by using eucalyptus liquefaction residues |
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| CN114950364A (en) * | 2022-05-23 | 2022-08-30 | 四川大学 | Biomass fast pyrolysis residue-based porous carbon sphere and preparation method and application thereof |
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| CN101054174A (en) * | 2007-04-05 | 2007-10-17 | 吉林大学 | Method of preparing biomass high specific surface micro-pore carbon material |
| CN101847481A (en) * | 2009-03-25 | 2010-09-29 | 中国科学院生态环境研究中心 | Novel process for preparing C-Fe shell-core magnetic active carbon by utilizing waste biomasses |
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| CN103657602A (en) * | 2013-12-03 | 2014-03-26 | 湖南大学 | Biological adsorbent, preparation method thereof, and application thereof to removal of methylene blue dye of waste water |
| CN103657602B (en) * | 2013-12-03 | 2015-11-18 | 湖南大学 | The purposes of biological adsorption agent, preparation method and removal methylene blue in waste dyestuff thereof |
| CN104492382A (en) * | 2013-12-06 | 2015-04-08 | 东华理工大学 | Preparation method of carboxylation hydrothermal biomass charcoal for remedying uranium-containing wastewater |
| CN105126755A (en) * | 2015-09-10 | 2015-12-09 | 哈尔滨工业大学宜兴环保研究院 | Novel magnetic active carbon and preparation method thereof |
| CN105439238A (en) * | 2015-12-11 | 2016-03-30 | 哈尔滨工业大学宜兴环保研究院 | Method for integrated treatment of dyeing wastewater by using magnetic activated carbon |
| CN105731452A (en) * | 2016-01-22 | 2016-07-06 | 青岛大学 | Active carbon electrode material as well as preparation method and application thereof |
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| CN107029535B (en) * | 2017-03-01 | 2020-02-11 | 沃邦环保有限公司 | Deodorization composition for culture manure treatment and application thereof |
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Application publication date: 20131127 |