CN105969412A - Method for ethanol synergetic improvement of carbonization degree of biomass hydrothermal charcoal - Google Patents
Method for ethanol synergetic improvement of carbonization degree of biomass hydrothermal charcoal Download PDFInfo
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- CN105969412A CN105969412A CN201610268052.6A CN201610268052A CN105969412A CN 105969412 A CN105969412 A CN 105969412A CN 201610268052 A CN201610268052 A CN 201610268052A CN 105969412 A CN105969412 A CN 105969412A
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- hydro
- seed
- ethanol
- arillus longan
- carbonization
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Classifications
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
- C10B53/00—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form
- C10B53/02—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form of cellulose-containing material
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
- C10B57/00—Other carbonising or coking processes; Features of destructive distillation processes in general
- C10B57/12—Applying additives during coking
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/30—Fuel from waste, e.g. synthetic alcohol or diesel
Abstract
The invention discloses a method for ethanol synergetic improvement of the carbonization degree of biomass hydrothermal charcoal, and belongs to the technical field of waste biomass carbonization high-value utilization. The method includes the following steps: cleanly washing and drying longan seeds, then crushing to obtain a longan seed powder with the particle size of less than 74 [mu]m, carrying out a hydrothermal reaction, adding ethanol in a hydrothermal reaction medium, and carrying out centrifugal separation, washing and drying and other ways, to obtain the longan seed-based hydrothermal charcoal. The used raw material is waste biomass and is low in price, so not only are the application value and the utilization rate of the longan seeds improved, but also a new source is provided for preparation of biomass hydrothermal charcoal; the preparation method has the advantages of environmental friendliness of the raw material, quick reaction, easy operation and good reproducibility; the longan seed-based hydrothermal charcoal prepared by adding ethanol has the advantages of black color and luster, high carbonization degree, high aromaticity, and good stability, can be widely used in the fields of preparation of activated carbon, new energy device electrode materials, catalyst carriers and the like.
Description
Technical field
The invention belongs to abandoned biomass carbonization high-value-use technical field, be specifically related to a kind of by adding the method that ethanol promotes biomass by hydro-thermal charcoal degree of carbonization.
Background technology
Carbon Materials preparation mainly includes the technology such as pyrolysis charring and hydro-thermal carbonization, and wherein, hydro-thermal charring process is a kind of its reaction condition gentleness, environmental protection, carbon sequestration rate height, environmental friendliness, simple emerging charcoal processing technology of technique.Hydro-thermal charcoal is the novel charcoal material that a kind of surface has the oxygen-containing functional groups such as abundant phenol, ether, carbonyl, quinone, carboxyl, anhydride, lactone, novel material or raw material can be formed further by physically or chemically activation, surface modification, the means such as supporting matrix or fertilizer that are blended, the aspects such as electrode material, catalyst carrier, soil remediation, water process and aquatic ecological restoration, medicine conveying, the charcoal base manure at novel energy-storing device have broad application prospects, visible, the synthesis of hydro-thermal charcoal and applied research have important scientific meaning and realistic price.The advantages such as hydro-thermal charring has that raw material is cheap and easy to get, synthesis technique energy-conserving and environment-protective, synthetic product and by-product environmental friendliness, consersion unit operation are simple, become the popular method of the Related Research Domain such as abandoned biomass carbonization in recent years and application.But, the most just due to hydro-thermal carbon surface, there is abundant oxygen-containing functional group, its stability of relative pyrolytic carbon is the highest, and when using as soil-repairing agent or fertilizer carrier, its life-span present in the soil is relatively short.Therefore, the stability by hydro-thermal charring process improvement lifting hydro-thermal charcoal is significant.
Abandoned biomass has the features such as source is wide, cheap, amount usable is big, can directly obtain, it is not necessary to through complicated pretreatment and chemical process, be the fourth-largest energy source type being only second to coal, oil, natural gas in the world from agricultural, forestry environment.Containing substantial amounts of lignin, cellulose, hemicellulose in biomass, traditional burning disposal not only wastes resource, also pollutes environment, and therefore, the abandoned biomass high-value-use technology of exploitation clean and effective is the most necessary.By the cheap abandoned biomass function Carbon Materials by eco-friendly mode high added value, both abandoned biomass decrement can have been reached, the purpose of abandoned biomass carbonization high-value-use can be realized again, utilize aspect to have great importance in the synthesis of functional Carbon Materials, abandoned biomass high level carbonization.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of lifting hydro-thermal charcoal degree of carbonization simple, efficient, eco-friendly, it is specially a kind of ethanol and works in coordination with the method promoting seed of Arillus Longan hydro-thermal charcoal degree of carbonization, the method is with abandoned biomass seed of Arillus Longan as raw material, water-ethanol mixing water thermal reaction medium is formed by adding ethanol, finally making the seed of Arillus Longan hydro-thermal charcoal degree of carbonization obtained be improved, the seed of Arillus Longan hydro-thermal charcoal color and luster prepared by the method is black, degree of carbonization is high, aromaticity is high, good stability.
The method promoting biomass by hydro-thermal charcoal degree of carbonization worked in coordination with by described a kind of ethanol, it is characterised in that comprise the following steps:
1) Feedstock treating: collect seed of Arillus Longan, cleans, and dries, uses portable Chinese medicine grinder to be ground into seed of Arillus Longan powder, standby；
2) hydro-thermal reaction: seed of Arillus Longan powder that mass ratio is 1:5:0-1:1:4, deionized water, ethanol are uniformly mixed, proceed in hydrothermal reaction kettle liner and seal hydrothermal reaction kettle, it is subsequently placed in 160 DEG C of-320 ° of DEG C of baking ovens reaction 4-48 hour, take out reactor, it is cooled to room temperature, obtains reactant mixture；
3) centrifugation and washing and drying: by step 2) reactant mixture proceed in centrifuge tube, be centrifuged successively separating, deionized water wash and drying, obtain seed of Arillus Longan base hydro-thermal charcoal.
The method promoting biomass by hydro-thermal charcoal degree of carbonization worked in coordination with by described a kind of ethanol, it is characterised in that in described step 1), seed of Arillus Longan is dried to moisture content less than 10%, seed of Arillus Longan powder particle be smaller in size than 74 μm.
The method promoting biomass by hydro-thermal charcoal degree of carbonization worked in coordination with by described a kind of ethanol, it is characterised in that described step 2) in seed of Arillus Longan powder, deionized water, the mass ratio of ethanol be 1:1:4.
Described a kind of ethanol work in coordination with promote biomass by hydro-thermal charcoal degree of carbonization method, it is characterised in that described step 2) in oven temperature be 260 °.
Described a kind of ethanol work in coordination with promote biomass by hydro-thermal charcoal degree of carbonization method, it is characterised in that described step 2) in the hydro-thermal reaction time be 12 hours.
The method promoting biomass by hydro-thermal charcoal degree of carbonization worked in coordination with by described a kind of ethanol, it is characterised in that carries out 3-4 centrifugation and deionized water wash in described step 3) successively, then dries, obtains seed of Arillus Longan base hydro-thermal charcoal.
Described a kind of ethanol work in coordination with promote biomass by hydro-thermal charcoal degree of carbonization method, it is characterised in that described step 2) ethanol be dehydrated alcohol.
The method have the advantages that
1. utilizing abandoned biomass for raw material to prepare biomass by hydro-thermal charcoal, turn waste into wealth, decrease the wasting of resources, improve using value and the utilization rate of seed of Arillus Longan, the preparation for biomass by hydro-thermal charcoal provides new source.
2. the present invention is first with seed of Arillus Longan as raw material, forms water-ethanol mixing water thermal reaction medium by adding ethanol, finally gives the seed of Arillus Longan base hydro-thermal charcoal that degree of carbonization is higher, the method raw material environmental protection, reaction operation quick, easy and favorable reproducibility.
3. the seed of Arillus Longan base hydro-thermal charcoal color and luster that the method for the present invention prepares is black, carbonizing degree is high, aromaticity is high, good stability.
4. the preparation method of the present invention can be widely used for activated carbon prepare, the field such as new energy devices electrode material and catalyst carrier.
Accompanying drawing explanation
Fig. 1 is seed of Arillus Longan powder particle scanning transmission electron microscope (TEM) figure that the present invention uses；
Fig. 2 is seed of Arillus Longan powder particle scanning electron microscope (SEM) figure that the present invention uses；
Fig. 3 be the practical seed of Arillus Longan powder of the present invention, embodiment 1 prepared seed of Arillus Longan base hydro-thermal charcoal and embodiment 5 prepared the Fourier infrared absorption spectrogram of seed of Arillus Longan base hydro-thermal charcoal；
Fig. 4 is prepared scanning electron microscope (SEM) figure obtaining seed of Arillus Longan base hydro-thermal charcoal of the embodiment of the present invention 1；
Fig. 5 is prepared scanning electron microscope (SEM) figure obtaining seed of Arillus Longan base hydro-thermal charcoal of the embodiment of the present invention 5；
Fig. 6 is the embodiment of the present invention 1 and the prepared X-ray diffractogram XRD obtaining seed of Arillus Longan base hydro-thermal charcoal of embodiment 5.
Detailed description of the invention
In conjunction with embodiments of the invention, the invention will be further described.
Embodiment 1
1) Feedstock treating: collect seed of Arillus Longan, cleans, and drying to moisture content is 7%, and the seed of Arillus Longan taking 100g drying uses portable Chinese medicine grinder to pulverize, and obtains the granular size seed of Arillus Longan powder less than 50 μm, sees Fig. 1-2；
2) hydro-thermal reaction: seed of Arillus Longan powder that mass ratio is 10g:50g:0g, deionized water, dehydrated alcohol are uniformly mixed, then proceed in the hydrothermal reaction kettle polytetrafluoroethyllining lining that volume is 100mL, seal hydrothermal reaction kettle, it is placed in 260 DEG C of baking ovens reaction 12 hours, take out reactor, it is cooled to room temperature, obtains reactant mixture；
3) centrifugation and washing and drying: by step 2) reactant mixture proceed in 100ml centrifuge tube, centrifugation, obtain bottom precipitation, then add deionized water toward 100ml to wash, centrifugation the most again, repeat the above steps 4 times, finally dries the product that obtains, obtains C/O ratio for 76.18/23.82 seed of Arillus Longan base hydro-thermal charcoal.
Embodiment 2
Step 2) in seed of Arillus Longan powder, deionized water, the mass ratio of dehydrated alcohol be 10g:40g:10g, in step 3) the seed of Arillus Longan base hydro-thermal charcoal that is improved of degree of carbonization；The other the same as in Example 1.
Embodiment 3
Step 2) in seed of Arillus Longan powder, deionized water, the mass ratio of dehydrated alcohol be 10g:30g:20g, in step 3) the seed of Arillus Longan base hydro-thermal charcoal that is improved of degree of carbonization；The other the same as in Example 1.
Embodiment 4
Step 2) in seed of Arillus Longan powder, deionized water, the mass ratio of dehydrated alcohol be 10g:20g:30g, in step 3) the seed of Arillus Longan base hydro-thermal charcoal that is improved of degree of carbonization；The other the same as in Example 1.
Embodiment 5
Step 2) in seed of Arillus Longan powder, deionized water, the mass ratio of dehydrated alcohol be 10g:10g:40g；Step 3) obtains the seed of Arillus Longan base hydro-thermal charcoal that C/O is 89.23/10.77；The other the same as in Example 1.
Embodiment 6
Step 2) in oven temperature be 180 DEG C；In step 3) or the seed of Arillus Longan base hydro-thermal charcoal that is improved of degree of carbonization；The other the same as in Example 1.
Embodiment 7
Step 2) in oven temperature be 200 DEG C；In step 3) or the seed of Arillus Longan base hydro-thermal charcoal that is improved of degree of carbonization；The other the same as in Example 1.
Embodiment 8
Step 2) in oven temperature be 220 DEG C；In step 3) or the seed of Arillus Longan base hydro-thermal charcoal that is improved of degree of carbonization；The other the same as in Example 1.
Embodiment 9
Step 2) in oven temperature be 240 DEG C；Step 3) obtains the seed of Arillus Longan base hydro-thermal charcoal that degree of carbonization is improved；The other the same as in Example 1.
Embodiment 10
Step 2) in oven temperature be 260 DEG C；Step 3) obtains the seed of Arillus Longan base hydro-thermal charcoal that degree of carbonization is improved；The other the same as in Example 1.
Embodiment 11
Step 2) in oven temperature be 280 DEG C；Step 3) obtains the seed of Arillus Longan base hydro-thermal charcoal that degree of carbonization is improved；The other the same as in Example 1.
The seed of Arillus Longan base hydro-thermal charcoal prepared by the present invention, through Fourier infrared absorption spectrum analysis, electron microscope scanning measures and X-ray diffraction analysis understands, water-ethanol mixing water thermal reaction medium is formed by adding ethanol, seed of Arillus Longan base hydro-thermal charcoal degree of carbonization can be made to be improved, selecting seed of Arillus Longan powder, deionized water, the mass ratio of dehydrated alcohol is 1:1:4, selecting temperature is 260 DEG C, and 12 hours selective response time, carbonizing degree is best.
Measure with the analysis of embodiment 1 with the seed of Arillus Longan base hydro-thermal charcoal of embodiment 5 acquisition and understand:
As shown in Figure 3, wherein a represents the absorption spectrum of the practical seed of Arillus Longan raw material of the present invention, b represents the prepared absorption spectrum obtaining seed of Arillus Longan base hydro-thermal charcoal in embodiment 1, c represents the prepared absorption spectrum obtaining seed of Arillus Longan base hydro-thermal charcoal in embodiment 5, owing to seed of Arillus Longan starting components is complicated, the absorption position relatively horn of plenty that its Fourier infrared absorption spectrum is corresponding, for seed of Arillus Longan raw material, 3250 cm-1The stretching vibration absworption peak that strong broad peak is great amount of hydroxy group and a small amount of amino at place, 2924 cm-1The peak at place is fatty CH2, the asymmetrical stretching vibration peak of-CH, 2854 cm-1The peak at place is fatty CH2, the symmetrical stretching vibration peak of-CH, 1694 cm-1Place's absworption peak is mainly C=O stretching vibration in carboxylic acid and absorbs, 1594 cm-1Place is the C=C of armaticity, C=O stretching vibration peak, the seed of Arillus Longan base hydro-thermal charcoal of embodiment 1 preparation is close with the part major absorbance peak position of raw material seed of Arillus Longan, but there is notable difference in the relative amount of chemical functional group, for the embodiment 5 adding ethanol, the organo-functional group of the seed of Arillus Longan base hydro-thermal charcoal obtained by embodiment 5 is (such as CH2,-CH, C=O etc.) absworption peak be remarkably reinforced, show that its aromaticity presents the trend of rising, visible, water-ethanol mixing water thermal reaction medium is formed by adding ethanol, the seed of Arillus Longan base hydro-thermal charcoal degree of carbonization prepared can be made to be improved.
Learn as Fig. 4-5 and relevant EDS collection of illustrative plates measure, embodiment 1 prepared the C/O ratio of seed of Arillus Longan base hydro-thermal charcoal for 76.18/23.82, the prepared C/O obtaining seed of Arillus Longan base hydro-thermal charcoal of embodiment 5 is 89.23/10.77, embodiment 5 is prepared into the charcoal oxygen ratio of seed of Arillus Longan base hydro-thermal charcoal and significantly improves, also explanation degree of carbonization improves, visible, form water-ethanol mixing water thermal reaction medium by adding ethanol, the seed of Arillus Longan base hydro-thermal charcoal degree of carbonization prepared can be made to be improved.
As shown in Figure 6, wherein a is the prepared X-ray diffractogram XRD obtaining seed of Arillus Longan base hydro-thermal charcoal of embodiment 1, b is the prepared X-ray diffractogram XRD obtaining seed of Arillus Longan base hydro-thermal charcoal of embodiment 5, substantially can be seen that, the diffraction maximum of prepared (002) crystal face obtaining seed of Arillus Longan base hydro-thermal charcoal of embodiment 5 strengthens, illustrate that in embodiment 5, the seed of Arillus Longan base hydro-thermal charcoal degree of carbonization of preparation is improved, visible, forming water-ethanol mixing water thermal reaction medium by adding ethanol, the seed of Arillus Longan base hydro-thermal charcoal degree of carbonization that can prepare is improved.
Claims (7)
1. the method promoting biomass by hydro-thermal charcoal degree of carbonization worked in coordination with by an ethanol, it is characterised in that comprise the following steps: 1) Feedstock treating: collect seed of Arillus Longan, clean, dry, use portable Chinese medicine grinder to be ground into seed of Arillus Longan powder, standby；
2) hydro-thermal reaction: seed of Arillus Longan powder that mass ratio is 1:5:0-1:1:4, deionized water, ethanol are uniformly mixed, proceed in hydrothermal reaction kettle liner and seal hydrothermal reaction kettle, it is subsequently placed in 160 DEG C of-320 DEG C of baking ovens reaction 4-48 hour, take out reactor, it is cooled to room temperature, obtains reactant mixture；
3) centrifugation and washing and drying: by step 2) reactant mixture proceed in centrifuge tube, be centrifuged successively separating, deionized water wash and drying, obtain seed of Arillus Longan base hydro-thermal charcoal.
The method promoting biomass by hydro-thermal charcoal degree of carbonization worked in coordination with by a kind of ethanol the most according to claim 1, it is characterised in that in described step 1), seed of Arillus Longan is dried to moisture content less than 10%, seed of Arillus Longan powder particle be smaller in size than 74 μm.
The method promoting biomass by hydro-thermal charcoal degree of carbonization worked in coordination with by a kind of ethanol the most according to claim 1, it is characterised in that described step 2) in seed of Arillus Longan powder, deionized water, the mass ratio of ethanol be 1:1:4.
A kind of ethanol the most according to claim 1 work in coordination with promote biomass by hydro-thermal charcoal degree of carbonization method, it is characterised in that described step 2) in oven temperature be 260 DEG C.
A kind of ethanol the most according to claim 1 work in coordination with promote biomass by hydro-thermal charcoal degree of carbonization method, it is characterised in that described step 2) in the hydro-thermal reaction time be 12 hours.
The method promoting biomass by hydro-thermal charcoal degree of carbonization worked in coordination with by a kind of ethanol the most according to claim 1, it is characterised in that carries out 3-4 centrifugation and deionized water wash in described step 3) successively, then dries, obtains seed of Arillus Longan base hydro-thermal charcoal.
A kind of ethanol the most according to claim 1 work in coordination with promote biomass by hydro-thermal charcoal degree of carbonization method, it is characterised in that described step 2) ethanol be dehydrated alcohol.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109554157A (en) * | 2018-11-30 | 2019-04-02 | 成都玉龙化工有限公司 | A kind of conduction fire retardant glue and preparation method thereof |
| CN112093791A (en) * | 2020-08-25 | 2020-12-18 | 江苏理工学院 | Preparation method and application of phosphorus-doped carbon material |
| CN115888644A (en) * | 2022-10-24 | 2023-04-04 | 广州大学 | Alcohol-modified peanut shell-based hydrothermal carbon material with high adsorption performance and preparation method thereof |
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| CN103359729A (en) * | 2013-08-01 | 2013-10-23 | 中国科学院西双版纳热带植物园 | Novel preparation method of mesoporous active carbon |
| CN103406096A (en) * | 2013-07-17 | 2013-11-27 | 国家纳米科学中心 | Nitrogen-doped porous carbon material, preparation method and use thereof |
| CN105143417A (en) * | 2012-12-19 | 2015-12-09 | 芬兰国家技术研究中心股份公司 | Process for the hydrothermal treatment of high molar mass biomaterials |
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2016
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20110017493A1 (en) * | 2009-07-22 | 2011-01-27 | Gibson Charles P | Carbon Microbeads with Hierarchical Structure |
| CN105143417A (en) * | 2012-12-19 | 2015-12-09 | 芬兰国家技术研究中心股份公司 | Process for the hydrothermal treatment of high molar mass biomaterials |
| CN103406096A (en) * | 2013-07-17 | 2013-11-27 | 国家纳米科学中心 | Nitrogen-doped porous carbon material, preparation method and use thereof |
| CN103359729A (en) * | 2013-08-01 | 2013-10-23 | 中国科学院西双版纳热带植物园 | Novel preparation method of mesoporous active carbon |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109554157A (en) * | 2018-11-30 | 2019-04-02 | 成都玉龙化工有限公司 | A kind of conduction fire retardant glue and preparation method thereof |
| CN112093791A (en) * | 2020-08-25 | 2020-12-18 | 江苏理工学院 | Preparation method and application of phosphorus-doped carbon material |
| CN115888644A (en) * | 2022-10-24 | 2023-04-04 | 广州大学 | Alcohol-modified peanut shell-based hydrothermal carbon material with high adsorption performance and preparation method thereof |
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Application publication date: 20160928 |