CN107603649B - It is a kind of richness ketone bio oil and rich magnesium active carbon preparation method - Google Patents
It is a kind of richness ketone bio oil and rich magnesium active carbon preparation method Download PDFInfo
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Abstract
The invention belongs to agriculture and forestry organic waste material fields of pyrolysis, and specifically disclose the preparation method of a kind of rich ketone bio oil and rich magnesium active carbon, are to be ground up, sieved agriculture and forestry organic waste material cleaning to obtain agriculture and forestry organic waste material powder；Then it by agriculture and forestry organic waste material powder and sea water mixing, and stirs and sufficiently obtains mixture, then mixture is dried to obtain the agriculture and forestry organic waste material powder after sea-changed；Modified agriculture and forestry organic waste material powder is sent into pyrolysis oven and carries out pyrolytic reaction acquisition pyrolytic carbon and volatile matter；The rich magnesium absorbent charcoal material with high-specific surface area and adsorption capacity is obtained after the washed drying of pyrolytic carbon, and rich ketone bio oil is obtained after volatile matter is cooling.Raw material sources of the present invention are extensive, and process is simple, and the rich ketone biology oil component being prepared is simple, and rich magnesium active carbon large specific surface area can efficiently remove the P elements in water body.
Description
Technical field
The invention belongs to agriculture and forestry organic waste material fields of pyrolysis, more particularly, to a kind of rich ketone bio oil and rich magnesium active carbon
Preparation method.
Background technique
The agriculture and forestry organic waste material in China is from a wealth of sources, and reserves are huge, and Land use systems mainly have directly burning, thermochemical study
With three kinds of approach of biochemical transformation, thermochemical method have simple process, be swift in response, high conversion rate, conversion strength greatly with
And it is easy to many advantages, such as industrializing.Pyrolysis is one kind of thermochemical method, using pyrolysis can be convenient by lignocellulosic
Biomass macromolecular is decomposed into various value products.But the bio oil complicated component that biomass is directly pyrolyzed, after
It is continuous to utilize difficulty.And charcoal has very big application in terms of agricultural and environmental protection as a kind of environmentally friendly material
Potentiality, but using biomass pyrolytic carbon come, adsorption efficiency too low in the prevalence of adsorbance when pollutant in adsorbed water body
The problems such as lower.
Before studies have shown that chemical modification can effectively improve biomass carbon to the absorption property of phosphorus.Such as publication number
A kind of magnesium-modified reed biomass carbon and its preparation method and application is disclosed in the Chinese patent literature of CN106000334A.Magnesium
The preparation step of modified reed biomass carbon are as follows: reed straw is ground up, sieved to obtain reed powder, by concentration be 0.5~
The MgCl of 0.75mol/L2Solution is mixed with reed powder, powder and MgCl2The mass volume ratio of solution is 0.1g/mL, through 80 DEG C
Pyrolysis charring after drying, pyrolysis temperature are 500~700 DEG C, time 1h, and heating rate is 10 DEG C/min, dry by washing
Modified reed biomass carbon is obtained after dry.The biomass carbon of this method preparation has been more than 100mg/g to the adsorbance of phosphorus, but should
Energy consumption is higher during method needs to consume a large amount of chemicals, and its pyrolysis prepares pyrolytic carbon, is pyrolyzed the gas of generation, oil etc.
Product does not utilize efficiently, and the utilization efficiency of biomass energy is lower.
Summary of the invention
Aiming at the above defects or improvement requirements of the prior art, the present invention provides a kind of rich ketone bio oil and rich magnesium activity
The preparation method of charcoal realizes same its object is to solve the further Utilizing question of agriculture and forestry organic waste material pyrolysis oil and pyrolytic carbon
When the single rich ketone bio oil of the prepared composition and rich magnesium absorbent charcoal material with high-specific surface area and adsorption capacity, pyrolytic process
In do not need the additions of other chemicals, it is environmentally protective, and greatly reduce preparation cost, improve the utilization of biomass energy
Efficiency.
To achieve the above object, according to one aspect of the present invention, a kind of preparation method of rich ketone bio oil is proposed, it should
Rich ketone bio oil is pyrogenically prepared using sea-changed agriculture and forestry organic waste material comprising following steps:
1) agriculture and forestry organic waste material is ground up, sieved to obtain agriculture and forestry organic waste material powder after deionized water is cleaned；
2) by agriculture and forestry organic waste material powder and sea water mixing obtained in step 1), and keep the two sufficiently mixed using magnetic agitation
To obtain mixture after conjunction, then mixture is dried to obtain the agriculture and forestry organic waste material powder after sea-changed；
3) modified agriculture and forestry organic waste material powder obtained in step 2) is sent into pyrolysis oven and carries out pyrolytic reaction, and will
The volatile matter that pyrolytic reaction generates is collected and cools down to obtain rich ketone bio oil.
As it is further preferred that the agriculture and forestry organic waste material is one of straw, cornstalk or rice husk or a variety of.
As it is further preferred that agriculture and forestry organic waste material is ground to 60~120 mesh in step 1), it is put into baking oven at 105 DEG C
It is spare after lower baking for 24 hours.
As it is further preferred that the mass volume ratio of agriculture and forestry organic waste material powder and seawater is 0.6~3g/ in step 2)
mL；The time of magnetic agitation is 4h；The temperature of drying is 105 DEG C, and the time is for 24 hours.
As it is further preferred that pyrolytic reaction described in step 3) carries out in a nitrogen atmosphere, the flow of nitrogen is
200mL/min, pyrolysis temperature are 450~850 DEG C, and heating rate is 10-20 DEG C/min, pyrolysis time 30min.
It gives up as it is further preferred that in step 3) after pyrolysis oven is warming up to pyrolysis temperature, then by modified agricultural
Gurry powder is sent into pyrolysis oven and carries out pyrolytic reaction.
As it is further preferred that containing 4- methyl -3- amylene -2- ketone, 3- in richness ketone bio oil obtained in step 3)
Methyl -4- amylene -2- ketone and 4- hydroxy-4-methyl-2-pentanone.
It is another aspect of this invention to provide that providing a kind of preparation method of rich magnesium active carbon, which is utilized
Sea-changed agriculture and forestry organic waste material is pyrogenically prepared comprising following steps:
1) agriculture and forestry organic waste material is ground up, sieved to obtain agriculture and forestry organic waste material powder after deionized water is cleaned；
2) by agriculture and forestry organic waste material powder and sea water mixing obtained in step 1), and keep the two sufficiently mixed using magnetic agitation
To obtain mixture after conjunction, then mixture is dried to obtain the agriculture and forestry organic waste material powder after sea-changed, the seawater
In contain MgCl2, concentration 1540mg/L；
3) modified agriculture and forestry organic waste material powder obtained in step 2) is sent into pyrolysis oven and carries out pyrolytic reaction to obtain
Obtain pyrolytic carbon；
4) pyrolytic carbon obtained in step 3) is obtained into rich magnesium active carbon after deionized water is washed and is dried.
In general, through the invention it is contemplated above technical scheme is compared with the prior art, mainly have below
Technological merit:
1. preparing rich ketone bio oil and rich magnesium active carbon using the pyrolysis of sea-changed agriculture and forestry organic waste material in method of the invention
Material realizes the higher value application of agriculture and forestry organic waste material, effectively improves the utilization efficiency of biomass castoff.
2. in method of the invention, during sea-changed agriculture and forestry organic waste material pyrolysis obtains rich ketone bio oil, without addition
Other chemicals, obtained bio oil are rich in ketone, and flavonoid content is up to 70%, and component is simple, and preparation process is environmentally protective, together
When greatly reduce preparation cost.
3. ketone component obtained in method of the invention (4- methyl -3- amylene -2- ketone, 3- methyl -4- amylene -2- ketone,
4- hydroxy-4-methyl-2-pentanone) there is very high selectivity, being conducive to the later period further purifies utilization.
4. acetic acid and other oxygenate contents are substantially reduced in bio oil obtained in method of the invention, life is reduced
The complexity of object oil component, the quality of bio oil have obtained very big promotion.
5. rich magnesium absorbent charcoal material obtained in method of the invention, magnesium content with higher and surface function abundant
Group, magnesium elements are mainly derived from seawater, take full advantage of the magnesium elements in seawater, and the mode of rich magnesium is better than usually using chemicals
Introduce the mode of magnesium elements.
6. pyrolysis gas by-product calorific value with higher, may be used as combustion gas obtained in method of the invention, realize
The comprehensive utilization of biomass pyrolysis product improves the utilization efficiency of biomass energy.
7. the raw material sources that the present invention uses during the preparation process are extensive, process is simple, and rich magnesium active carbon ratio is prepared
Surface area is big, specific surface area > 200m2/ g can efficiently remove the P elements in water body.
Detailed description of the invention
Fig. 1 is the gas of the rich ketone bio oil provided in an embodiment of the present invention using the pyrolysis preparation of sea-changed agriculture and forestry organic waste material
Phase chromatography-mass spectroscopy test result figure；
Fig. 2 is the richness provided in an embodiment of the present invention for being pyrolyzed preparation at different temperatures using sea-changed agriculture and forestry organic waste material
The content balance figure of ketone and acetic acid substance in ketone bio oil；
Fig. 3 is the rich magnesium active carbon provided in an embodiment of the present invention using the pyrolysis preparation of sea-changed agriculture and forestry organic waste material
XRD spectra；
Fig. 4 is a kind of flow chart of rich ketone bio oil preparation method provided in an embodiment of the present invention.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.As long as in addition, technical characteristic involved in the various embodiments of the present invention described below
Not constituting a conflict with each other can be combined with each other.
The preparation method and a kind of preparation method of rich magnesium active carbon of a kind of rich ketone bio oil provided in an embodiment of the present invention,
Wherein, rich ketone bio oil is pyrogenically prepared using sea-changed agriculture and forestry organic waste material, as shown in figure 4, it includes the following steps:
1) agriculture and forestry organic waste material is ground up, sieved to obtain agriculture and forestry organic waste material powder after deionized water is cleaned；
2) by agriculture and forestry organic waste material powder and sea water mixing obtained in step 1), and keep the two sufficiently mixed using magnetic agitation
To obtain mixture after conjunction, then mixture is dried to obtain the agriculture and forestry organic waste material powder after sea-changed, wherein seawater
In main component be MgCl2, concentration 1540mg/L, the i.e. MgCl containing 1540mg in one liter of seawater2；
3) modified agriculture and forestry organic waste material powder obtained in step 2) is sent into pyrolysis oven and carries out pyrolytic reaction, be pyrolyzed
Pyrolytic carbon can be obtained in reaction, and pyrolytic carbon can be used for preparing rich magnesium active carbon, and can generate volatile matter during the reaction, will wave
Hair point, which is collected and cooled down, can be obtained rich ketone bio oil.
Flavonoid content is up to 70% in the rich ketone bio oil that this method prepares, and contains 4- first in rich ketone bio oil
Base -3- amylene -2- ketone, 3- methyl -4- amylene -2- ketone and 4- hydroxy-4-methyl-2-pentanone, it is modified for obtaining principle
Agriculture and forestry organic waste material powder heating pyrolysis when, cellulose therein, hemicellulose, the structures such as lignin under the catalysis of magnesium elements,
By dehydration, depolymerization and interaction between generate the volatile matter for being rich in ketone product, and volatile matter is mixed by ice water
It is condensed when object and is collected into the bio oil of rich ketone.
And rich magnesium active carbon is pyrogenically prepared also with sea-changed agriculture and forestry organic waste material, is the heat for obtaining pyrolytic reaction
Solution charcoal is handled to prepare rich magnesium active carbon comprising following steps:
1) agriculture and forestry organic waste material is ground up, sieved to obtain agriculture and forestry organic waste material powder after deionized water is cleaned；
2) by agriculture and forestry organic waste material powder obtained in step 1) and seawater with different solid ratio (mass/volume) hybrid infusion
Processing, and both made after being sufficiently mixed using magnetic agitation to obtain mixture, then mixture is dried to evaporate moisture,
And then the agriculture and forestry organic waste material powder after sea-changed is obtained, wherein the main component of seawater is MgCl2, concentration 1540mg/
L；
3) modified agriculture and forestry organic waste material powder obtained in step 2) is sent into pyrolysis oven and carries out pyrolytic reaction to obtain
Pyrolytic carbon is obtained, the magnesium chloride in pyrolytic process in modified agriculture and forestry organic waste material powder, which decomposes to react, generates magnesium oxide particle
It is attached to the surface of charcoal, the volatile matter for being pyrolyzed generation is collected and cools down the rich ketone bio oil of acquisition；
4) pyrolytic carbon obtained in step 3) is obtained into rich magnesium active carbon after deionized water is washed and is dried.
Further, the agriculture and forestry organic waste material is one of straw, cornstalk or rice husk or a variety of.Further,
Agriculture and forestry organic waste material powder is that agriculture and forestry organic waste material is ground to 60~120 mesh, is then placed in baking oven to dry at 105 DEG C and make afterwards for 24 hours
It is standby to obtain.
Preferably, the mixed mass volume ratio of agriculture and forestry organic waste material powder and seawater is 0.6~3g/mL；And magnetic agitation
Time be 4h；The temperature of drying is 105 DEG C, and the time is for 24 hours.
Preferably, pyrolytic reaction carries out in a nitrogen atmosphere in step 3), and the flow of nitrogen is 200mL/min, pyrolysis temperature
Degree is 450~850 DEG C, and heating rate is 10-20 DEG C/min, pyrolysis time 30min.When pyrolytic reaction, first by pyrolysis oven liter
To pyrolysis temperature, then modified agriculture and forestry organic waste material powder is quickly pushed into the pyrolysis oven for having risen to pyrolysis temperature, is pyrolyzed
30min, after pyrolysis, obtained pyrolytic carbon takes out after being cooled to room temperature under nitrogen atmosphere.
The rich magnesium active carbon that this method prepares has pore structure abundant (specific surface area > 200m2/ g), and by
It is attached with small magnesium oxide particle in activated carbon surface, therefore can promote the surface of charcoal that proton occurs in aqueous solution
Change, keep the surface of charcoal positively charged, electrostatic attraction occurs with the phosphate radical in solution, improves its absorption property, therefore the richness
Magnesium active carbon has efficient absorption property, is with a wide range of applications in terms of handling phosphorous eutrophication water.
The following are specific embodiments of the present invention.
Embodiment 1
Cornstalk crushing is sized to 60-120 mesh, and is put into baking oven to dry at 105 DEG C and obtains cornstalk powder for 24 hours,
Cornstalk powder is mixed from seawater with different solid-to-liquid ratios (3,1.5,1,0.75,0.6), and is stirred using magnetic agitation
4h is so that cornstalk powder is sufficiently mixed the mixture for obtaining the cornstalk powder and seawater that are uniformly mixed with seawater, by cornstalk
The mixture of powder and seawater dries at 105 DEG C obtains modified cornstalk powder for 24 hours；It the use of diameter is 45mm, length is
The fixed bed reactors (i.e. pyrolysis oven) of 60mm are pyrolyzed, and reactor is heated to refer to the heating rate of 10-20 DEG C/min
Determine 550 DEG C of temperature, 2g modified biomass (i.e. modified cornstalk powder) is rapidly feeding in the middle part of reactor, the reaction time is
30min is pyrolyzed modified biomass sufficiently, and pyrolytic reaction obtains pyrolytic carbon and generates volatile matter, is pyrolyzed in nitrogen atmosphere
It carries out, nitrogen flow 200mL/min.Wherein, volatiles are brought into condenser by nitrogen, cooling by mixture of ice and water
Liquid product is obtained, which is rich ketone bio oil, and the flavonoid content in rich ketone bio oil is up to 70%.Pyrolysis generates
Pyrolysis coke (i.e. pyrolytic carbon) after natural cooling after washing, be put into 105 DEG C of oven dryings for 24 hours, obtain rich magnesium activity
The active carbon of charcoal, preparation has more developed pore structure (specific surface area > 200m2/ g), higher magnesium content (reaches as high as
18.69wt.%), it can be applied to adsorbing domain.In addition, collecting the gas that pyrolysis generates, combustion gas use can be used as.
Fig. 1 is GC-MS (gas chromatograph-mass spectrometer (GC-MS)) spectrogram of rich ketone bio oil manufactured in the present embodiment, such as Fig. 1 institute
Show, the ketone in rich ketone bio oil is mainly 4- methyl -3- amylene -2- ketone, 3- methyl -4- amylene -2- ketone, 4- hydroxyl -4- first
Base -2 pentanone etc., acetic acid and other product assays reduce in bio oil, reduce the complexity of biological oil component, bio oil
Quality has obtained very big promotion.
Embodiment 2
The solid-liquid mixing ratio for controlling cornstalk and seawater is 2:5, and research pyrolysis temperature is living for rich ketone bio oil and rich magnesium
The influence of property charcoal, pyrolysis temperature is respectively 450 DEG C, 550 DEG C, 650 DEG C, 750 DEG C, 850 DEG C, and other conditions are same as Example 1.
As shown in Fig. 2, under 450 DEG C, 550 DEG C, 650 DEG C, 750 DEG C and 850 DEG C of pyrolysis temperature, containing height in obtained bio oil
The letones of content, and acetic acid content is lower, and the higher letones content of temperature is higher, acetic acid content is lower, and temperature reaches
When to 850 DEG C, the content of letones tends towards stability.Rich magnesium active carbon prepared by the present invention has high-specific surface area, and has
Higher content of magnesium, as shown in figure 3, magnesium is predominantly in the form of MgO and Mg (OH) in active carbon2, chlorine in biomass
Change magnesium decomposition in pyrolysis and generate MgO and HCl, MgO is attached to the surface of charcoal, finally carries out deionization washing to charcoal
When washing, part MgO meets water and is changed into Mg (OH)2。
To sum up, the present invention is pyrolyzed by sea-changed agriculture and forestry organic waste material, can significantly improve bio oil small molecular ketone
Content, obtain the biological oil product rich in ketone；Pyrolytic carbon is available to have high-ratio surface after washing and drying treatment
Long-pending and adsorption capacity rich magnesium absorbent charcoal material.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should all include
Within protection scope of the present invention.
Claims (7)
1. a kind of preparation method of richness ketone bio oil, which is characterized in that the richness ketone bio oil utilizes sea-changed agriculture and forestry organic waste material
It is pyrogenically prepared comprising following steps:
1) agriculture and forestry organic waste material is ground up, sieved to obtain agriculture and forestry organic waste material powder after deionized water is cleaned；
2) by agriculture and forestry organic waste material powder and sea water mixing obtained in step 1), and both made after being sufficiently mixed using magnetic agitation
To obtain mixture, then mixture is dried to obtain the agriculture and forestry organic waste material powder after sea-changed；
3) modified agriculture and forestry organic waste material powder obtained in step 2) is sent into pyrolysis oven and carries out pyrolytic reaction, and will pyrolysis
The volatile matter that reaction generates is collected and cools down to obtain rich ketone bio oil, and 4- methyl -3- amylene-is contained in the richness ketone bio oil
2- ketone, 3- methyl -4- amylene -2- ketone and 4- hydroxy-4-methyl-2-pentanone.
2. the preparation method of richness ketone bio oil according to claim 1, which is characterized in that the agriculture and forestry organic waste material is wheat
One of stalk, cornstalk or rice husk are a variety of.
3. the preparation method of richness ketone bio oil according to claim 1 or 2, which is characterized in that agricultural are discarded in step 1)
Object is ground to 60~120 mesh, is put into baking oven spare after drying at 105 DEG C for 24 hours.
4. the preparation method of richness ketone bio oil according to claim 1, which is characterized in that agriculture and forestry organic waste material powder in step 2)
The mass volume ratio of end and seawater is 0.6~3g/mL；The time of magnetic agitation is 4h；The temperature of drying is 105 DEG C, and the time is
24h。
5. the preparation method of richness ketone bio oil according to claim 1, which is characterized in that pyrolytic reaction described in step 3)
It carries out in a nitrogen atmosphere, the flow of nitrogen is 200mL/min, and pyrolysis temperature is 450~850 DEG C, heating rate 10-20
DEG C/min, pyrolysis time 30min.
6. the preparation method of richness ketone bio oil according to claim 1, which is characterized in that heat up in step 3) in pyrolysis oven
To pyrolysis temperature, then modified agriculture and forestry organic waste material powder is sent into pyrolysis oven and carries out pyrolytic reaction.
7. a kind of preparation method of rich magnesium active carbon, which is characterized in that the rich magnesium active carbon utilizes sea-changed agriculture and forestry organic waste material
It is pyrogenically prepared comprising following steps:
1) agriculture and forestry organic waste material is ground up, sieved to obtain agriculture and forestry organic waste material powder after deionized water is cleaned；
2) by agriculture and forestry organic waste material powder and sea water mixing obtained in step 1), and both made after being sufficiently mixed using magnetic agitation
To obtain mixture, then mixture is dried to obtain the agriculture and forestry organic waste material powder after sea-changed, is contained in the seawater
There is MgCl2, concentration 1540mg/L；
3) modified agriculture and forestry organic waste material powder obtained in step 2) is sent into pyrolysis oven and carries out pyrolytic reaction to obtain heat
Solve charcoal；
4) pyrolytic carbon obtained in step 3) is obtained into rich magnesium active carbon after deionized water is washed and is dried, the rich magnesium active carbon
With pore structure abundant, specific surface area > 200m2/ g, magnesium content is high, reaches 18.69wt.%, and rich magnesium activated carbon surface
It is attached with magnesium oxide particle, the surface of charcoal can be promoted to protonate in aqueous solution, makes the surface band of charcoal just
Electrostatic attraction occurs for the phosphate radical in charge, with solution, improves its absorption property.
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| CN109650388A (en) * | 2019-01-21 | 2019-04-19 | 武汉大学 | A kind of method and its application preparing biomass-based functional activity Carbon Materials using concentrated seawater auxiliary |
| CN113941314B (en) * | 2021-11-06 | 2024-01-30 | 闽江学院 | Seawater modified biochar and preparation method and application thereof |
| CN114130357A (en) * | 2021-12-03 | 2022-03-04 | 海西州盐化工产品质量检验检测中心 | Preparation method and application of salt lake old brine modified biochar |
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| CN105377958B (en) * | 2013-05-03 | 2019-01-01 | 威尔迪亚公司 | Method for handling ligno-cellulosic materials |
| CN106000334A (en) * | 2016-05-12 | 2016-10-12 | 浙江大学 | Modified reed biomass charcoal and preparing method and application thereof |
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