CN108689407A - A kind of technique that binder pressed active carbon is exempted from abandoned biomass preparation - Google Patents
A kind of technique that binder pressed active carbon is exempted from abandoned biomass preparation Download PDFInfo
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- CN108689407A CN108689407A CN201810670041.XA CN201810670041A CN108689407A CN 108689407 A CN108689407 A CN 108689407A CN 201810670041 A CN201810670041 A CN 201810670041A CN 108689407 A CN108689407 A CN 108689407A
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- active carbon
- biomass
- binder
- pressed active
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
- C01B32/324—Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/342—Preparation characterised by non-gaseous activating agents
- C01B32/348—Metallic compounds
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/354—After-treatment
Abstract
The features such as pressed active carbon is because of large specific surface area, controllable shape has been applied in numerous areas such as food, medicine, chemical industry, environmental protection.Existing pressed active carbon is that powder active carbon is molded preparation by binder mostly.Powder active carbon is expensive, and in addition binder can not only reduce the adsorption effect of pressed active carbon, and there are secondary pollution problems.Therefore, cheap, environmentally protective binder pressed active carbon of exempting from is developed to have important practical significance.Abandoned biomass is modified processing by the present invention under given conditions, obtains by the method chemically or physically activated described exempting from binder pressed active carbon after modified biomass moulding.Compared with traditional pressed active carbon, pressed active carbon prepared by the present invention is not necessarily to binder, therefore have many advantages, such as that preparation process is simple, at low cost, renewable, environmentally protective using abandoned biomass as raw material.
Description
Technical field
The present invention relates to abandoned biomass processing to dispose, and belongs to the solid waste of environmental protection and comprehensive utilization of resources field
Object recycling new technology is particularly suitable for the high added value recycling of the abandoned biomass such as stalk, the bamboo scraps of enormous amount
It utilizes.
Background technology
Compared with powder active carbon, pressed active carbon has controllable size and shape, there is higher heap density and intensity
And without dust pollution.Meanwhile the high intensity and machinability of pressed active carbon can meet the need of the multiple use of different industries
It asks.In addition, pressed active carbon is easily recycled, regeneration.Feature due to its protrusion and wide application prospect, pressed active carbon is
By more and more extensive concern, become the hot spot studied both at home and abroad.
Pressed active carbon is mainly prepared by powder active carbon and binder by compression molding.Production cost is high and is molded
Properties of Activated Carbon is relatively low be limit its in practice large-scale application the main reason for.Currently, powder active carbon is mainly by coal
Or prepared by the fossil energies such as oil, production cost is relatively high.Binder is mainly organic used in powder active carbon forming process
Class and inorganic two major classes.Either inorganic binder or organic binder can all lead to the specific surface of activated carbon after molding
Product declines.In addition, needing binder and powdered carbon being heated to certain temperature during powder active carbon molding bonded, so energy consumption
It is higher;Finally, the pressed active carbon prepared by organic binder is easy to get the pressed active carbon of high specific surface area, therefore
Mostly use organic binder greatly in practical forming process, but organic binder is easy degradation aging, and catabolite is deposited
In secondary pollution risk.
The present invention is prepared for exempting from binder pressed active carbon using abandoned biomass as raw material by being modified to biomass,
The pressed active carbon has green, environmental protection, lower-price characteristic.The same of binder pressed active carbon is exempted from abandoned biomass preparation
When also be a large amount of abandoned biomass have found an effective high value added utilization technology.
Invention content
The present invention is existing for high, powder active carbon binder processability difference of existing powder active carbon manufacturing cost etc.
Shape is established a kind of prepared with abandoned biomass and exempts from binder movable forming in conjunction with the advantage that China's abandoned biomass is resourceful
The new process of property charcoal.Concrete technology is characterized in that:After abandoned biomass, water are mixed in certain proportion, by gained mixture
Be put into hydrothermal reactor and carry out hydro-thermal process under certain condition, be cooled to room temperature rear hydro-thermal biomass and chemical activating agent at
Type, heat treatment either vapor or CO after hydro-thermal biomass straight forming2It activates and exempts from binder pressed active carbon up to described.
The abandoned biomass is in terms of butt, and the quality proportioning with the water being added when hydro-thermal process is 1:1-1:10
Between.
The hydro-thermal process temperature is preferably 150-300 DEG C, and processing time is 30-90 minutes.
Biomass crushed after being dried is to 80-200 mesh after the hydro-thermal process.
The compression molding be hydro-thermal biomass after crushing with activator (zinc chloride, potassium hydroxide etc.) according to 1:
1-1:5 mass ratios mix, compression molding at room temperature, are demoulded after molding pressure 3-30Mpa, dwell time 0.5-10min;
Or the hydro-thermal biomass after crushing is molded directly into type, molding pressure 3-30Mpa, dwell time 0.5- at room temperature
It is demoulded after 10min.
The activation is in inert atmosphere by the molding hydro-thermal biomass containing activator with 1-20 DEG C/min heating speed
Rate is heated to 400-900 DEG C and keeps 30min, and washing and drying obtains exempting from binder molding after being cooled to room temperature in inert atmosphere
Activated carbon;Or straight forming hydro-thermal biomass is heated to 400-900 DEG C in inert atmosphere with 1-20 DEG C/min heating rates
It is 10-100cm to convert inert gas to flow velocity afterwards3The vapor or CO of/min2Gas, and 30min is kept, in vapor
Or CO2Rear washing and drying is cooled to room temperature in atmosphere to obtain exempting from binder pressed active carbon.
What the process described above was prepared exempts from binder pressed active carbon.
Advantages of the present invention is as follows:
The present inventor's creativeness has selected the hydrothermal modification treatment to abandoned biomass.The processing can reach simultaneously
To following purpose:1. the range (uniforming) of abandoned biomass particle size distribution can be reduced by hydro-thermal process, generate bright
Aobvious pore structure, relatively uniform particle size, increased pore structure make hydro-thermal biomass particle particle in forming process
Between physical force increase;2. introducing abundant oxygen-containing polar functional group (such as phenolic hydroxyl group, carboxyl, aldehyde in biological surface
Base, lactone group etc.), these polar functional groups make not only to generate high Van der Waals force, dispersion force, Er Qiebiao during particle former
It can be molded by forming forces such as liquid bridge, hydrogen bonds between functional group's (mainly oxygen-containing polar functional group) in face;3. in biomass
The furane resins structure and polyphenol structure sheet formed after three big chemical constituent hemicelluloses, cellulose and lignin hydrothermal modification
Body is exactly extraordinary natural adhesive;4. hydro-thermal process can remove the nonpolar long-chain hydrocarbon structure of biological surface, improve
Molecular force in forming process between particle;So by hydro-thermal process can greatly promote biomass processability (at
Type power is as shown in Figure 1).
Biomass (butt) and the mixed proportion of water are 1 in water-heat process:1-1:Between 10.Too low water addition can be led
Cause it is biomass carbonated be not thorough, and too high water addition can not only greatly increase the energy consumption of hydro-thermal process, but also generate a large amount of
Waste water, increase carrying capacity of environment.
Hydro-thermal process temperature is 150-300 DEG C, and processing time is 30-90 minutes.Too low temperature and too short time meeting
Cause the pore structure of biomass undeveloped and surface functional group does not enrich;And too high reaction temperature and too long of reaction time are not
The energy consumption of processing procedure can only be increased and biomass central hole structure can be caused after hydro-thermal process to cave in and surface functional group
It falls off.
Biomass crushed after being dried is to 80-200 mesh after hydro-thermal process.Too thin granularity increases the energy consumption of crushing process, and
Too big particle is difficult to form strong interaction between adjacent particles, it is difficult to be molded due to too big in mold process void.
Hydro-thermal biomass is with chemical activating agent mixed proportion preferably 1:1-1:Between 5, too low activator addition pore-creating
Effect is poor, and the carbon content that too high activator can reduce pressed active carbon equally reduces pore structure;
Molding refers to hydro-thermal biomass hybrid activator or hydro-thermal biomass is molded directly into type, and molding pressure is preferably 3-
30MPa, dwell time are preferably 0.5-10min.The time of too high pressure and length increases processing procedure energy consumption;And it is too low
Pressure and too short time can cause the mechanical strength of pressed active carbon too low;In addition hydro-thermal biomass and chemical activating agent is mixed
Composition and division in a proportion example preferably 1:1-1:5, chemical activating agent includes potassium hydroxide, zinc chloride etc., and wherein hydro-thermal biomass is mixed with activator
Mode can directly solid-state physics mixed-forming or hydro-thermal biomass mixed with activator solution after again by water evaporation aftershaping.
The formed body of hybrid activator heats in inert atmosphere is heated to 400-900 DEG C with 1-20 DEG C/min heating rates
And 30min-60min is kept, it is cooled to room temperature rear washing and drying and exempts from binder pressed active carbon to obtain the final product;Heat treatment temperature is preferred
400-900 DEG C, retention time preferred 30-60min.Too low temperature and too short time can cause to activate insufficient, pore structure
It is undeveloped;And too high temperature and long time can cause pore structure to be caved in, and increase processing procedure energy consumption.
Molding hydro-thermal biomass heats in inert atmosphere, after being heated to 400-900 DEG C with 1-20 DEG C/min heating rates
Convert inert gas to vapor or CO2Gas simultaneously keeps 30min, vapor and CO2The preferred 10-100cm of flow velocity3/min
Between.Vapor or CO2As physically activated dose too it is low can cause to activate it is insufficient, and it is too high micropore can be caused to reduce, reduce
Specific surface area, while too high temperature can cause the mechanical performance of pressed active carbon to reduce.
Prepared by the present invention exempts from binder pressed active carbon with reproducible abandoned biomass such as stalk, leaf, bamboo scraps etc.
It prepares, has the characteristics that at low cost, environmental-friendly for raw material.
With reference to the accompanying drawings of the specification and the embodiment content that the present invention is further explained.
Description of the drawings
Fig. 1 hydrothermal modifications promote the principle schematic of biomass moulding.
Fig. 2 abandoned biomass prepares the technological process of production schematic diagram for exempting from binder pressed active carbon.
Specific implementation mode
The present invention uses reproducible abandoned biomass such as lignocellulose biomass stalk (maize straw, cotton stalk
Deng), leaf, bamboo scraps etc. and non-wood cellulosic biomass such as feces of livestock and poultry (pig manure, chicken manure, cow dung etc.), municipal sludge, water
Algae etc. prepares for raw material.
Embodiment 1
1. material prepares
Abandoned biomass uses cotton stalk, stalk crushed after being dried spare to 80 mesh;
2. the preparation of pressed active carbon
1) by cotton stalk (butt), water with 1:5 ratio is sufficiently mixed;
2) after mixture is transferred to hydrothermal reaction kettle, sealing;
3) reaction kettle is heated to 220 DEG C of progress hydro-thermal process, stops heating, natural cooling after hydrothermal conditions 60min
To room temperature;
4) mixture obtains solid product after carrying out centrifugation solid waste separation in reaction kettle;
5) after solid product drying at room temperature with potassium hydroxide according to mass ratio 1:2 are sufficiently mixed (solid-state physics mixing);
6) it is demoulded (cylindrical long 2cm, diameter 1.5cm) after keeping 1min under molding pressure 5Mpa pressure after mixing;
7) formed body is heated to 700 DEG C in nitrogen atmosphere with 10 DEG C/min heating rates, keeps after 30min in nitrogen atmosphere
It encloses and is cooled to room temperature washing and drying and exempts from binder pressed active carbon to obtain the final product.
3. the performance measurement of pressed active carbon
1) specific surface area is carried out using nitrogen adsorption-desorption method.Pressed active carbon takes off under the conditions of 150 DEG C before absorption
Gas 5h;
2) mechanical strength tests compression strength on universal testing machine.
3) analysis result is as shown in table 1.
Embodiment 2
1. material prepares
Abandoned biomass uses bamboo scraps stalk, bamboo scraps crushed after being dried spare to 80 mesh;
2. the preparation of pressed active carbon
1) by bamboo scraps (butt), water with 1:4 ratio is sufficiently mixed;
2) after mixture is transferred to hydrothermal reaction kettle, sealing;
3) reaction kettle is heated to 250 DEG C of progress hydro-thermal process, stops heating, natural cooling after hydrothermal conditions 40min
To room temperature;
4) mixture obtains solid product after carrying out centrifugation solid waste separation in reaction kettle;
5) after solid product drying at room temperature with potassium hydroxide according to mass ratio 1:3 are sufficiently mixed (potassium hydroxide wiring solution-forming
Mix afterwards), 80 DEG C of dry 12h after mixing;
6) it keeps demoulding (cylindrical long 2cm, diameter 1.5cm) after 0.5min under molding pressure 4Mpa pressure after drying;
7) formed body is heated to 800 DEG C in nitrogen atmosphere with 10 DEG C/min heating rates, and keeps after 30min in nitrogen
Atmosphere is cooled to room temperature, and washing and drying exempts from binder pressed active carbon to obtain the final product.
3. the performance measurement of pressed active carbon is same as Example 1.
Analysis result is as shown in table 1.
Embodiment 3
1. material prepares
Abandoned biomass uses bamboo scraps, bamboo scraps crushed after being dried spare to 80 mesh;
2. the preparation of pressed active carbon
1) by bamboo scraps (butt), water with 1:4 ratio is sufficiently mixed;
2) after mixture is transferred to hydrothermal reaction kettle, sealing;
3) reaction kettle is heated to 250 DEG C of progress hydro-thermal process, stops heating, natural cooling after hydrothermal conditions 40min
To room temperature;
4) mixture obtains solid product and drying after carrying out centrifugation solid waste separation in reaction kettle;
5) it keeps demoulding (cylindrical long 2cm, diameter 1.5cm) after 0.5min under molding pressure 4Mpa pressure after drying;
7) nitrogen is changed to CO by formed body after being heated to 800 DEG C in nitrogen atmosphere with 10 DEG C/min heating rates2, CO2Stream
Speed is 100cm3In CO after/min, holding 30min2Atmosphere is cooled to room temperature, and washing and drying exempts from binder pressed active carbon to obtain the final product.
3. the performance measurement of pressed active carbon is same as Example 1.
Analysis result is as shown in table 1.
Prepared by 1. present invention of table exempts from the specific surface area and compression strength of binder pressed active carbon.
| Embodiment | Specific surface area (m2/g) | Compression strength (MPa) |
| 1 | 826 | 5 |
| 2 | 896 | 4 |
| 3 | 758 | 4 |
As it can be seen from table 1 binder molding charcoal of exempting from prepared by the present invention has very high specific surface area and machine
Tool intensity.In addition, pressed active carbon prepared by the present invention is using abandoned biomass as raw material, have at low cost, environmentally protective excellent
Point.
Claims (7)
1. a kind of abandoned biomass prepares the technique for exempting from binder pressed active carbon, it is characterised in that:By abandoned biomass and water
After certain ratio mixing, gained mixture is put into hydrothermal reactor and carries out hydrothermal modification under certain condition, is cooled to room
Isolated hydro-thermal biomass after temperature, then hydro-thermal biomass through crushing, compression molding, activation obtain it is described exempt from binder at
Type activated carbon.
2. a kind of abandoned biomass according to claim 1 prepares the technique for exempting from binder pressed active carbon, it is characterized in that:
The biomass is in terms of butt, and the quality proportioning for the water that when hydro-thermal process is added is 1:1-1:Between 10.
3. a kind of abandoned biomass according to claim 1-2 any one prepares the work for exempting from binder pressed active carbon
Skill, it is characterized in that:The hydro-thermal process temperature is 150-300 DEG C, and processing time is 30-90 minutes.
4. a kind of abandoned biomass according to claim 1-3 any one prepares the work for exempting from binder pressed active carbon
Skill, it is characterized in that:By biomass crushed after being dried to 50-200 mesh after hydro-thermal process.
5. a kind of abandoned biomass prepares the work for exempting from binder pressed active carbon according to any one of claims 1-4
Skill, it is characterized in that:By the hydro-thermal biomass after crushing with activator (zinc chloride, potassium hydroxide etc.) according to 1:1-1:10 ratios are mixed
It closes, compression molding at room temperature, is demoulded after molding pressure 3-30Mpa, dwell time 0.5-10min;Or it will be after crushing
Hydro-thermal biomass is molded directly into type at room temperature, is demoulded after molding pressure 3-30Mpa, dwell time 0.5-10min.
6. a kind of abandoned biomass according to claim 1-5 any one prepares the work for exempting from binder pressed active carbon
Skill, it is characterized in that:Molding hydro-thermal biomass containing activator is heated in inert atmosphere with 1-20 DEG C/min heating rates
400-900 DEG C and 30min is kept, washing and drying after postcooling to room temperature;Or straight forming hydro-thermal biomass is in inert atmosphere
In be heated to 400-900 DEG C with 1-20 DEG C/min heating rates after by inert gas be converted into flow velocity be 10-100cm3/ min water
Steam or CO2Gas simultaneously keeps 30min, is cooled to room temperature rear washing and drying.
7. what the method described in claim 1-6 any one was prepared exempts from binder pressed active carbon.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110182801A (en) * | 2019-04-01 | 2019-08-30 | 复旦大学 | A method of granular activated carbon is prepared with biomass |
| CN110299522A (en) * | 2019-06-26 | 2019-10-01 | 陕西科技大学 | A kind of preparation method of the biomass porous carbon nano-electrode material of high capacity sodium-ion battery Fluorin doped |
| CN110479226A (en) * | 2019-08-30 | 2019-11-22 | 郑州大学 | A kind of clay mineral/agricultural abandoned biomass compound sewage inorganic agent, preparation method and application |
| CN112340730A (en) * | 2020-11-24 | 2021-02-09 | 海南大学 | Preparation method of microporous carbon-rich material based on carboxylation anchoring effect |
| CN113563011A (en) * | 2021-08-03 | 2021-10-29 | 宁波瑞能环境能源技术有限公司 | Novel building energy-saving material and preparation method thereof |
| CN113891852A (en) * | 2019-03-29 | 2022-01-04 | 阿玛蒂克斯控制公司 | Method for producing highly activated, monolithic reticulated biochar electrodes |
| CN116254124A (en) * | 2022-11-01 | 2023-06-13 | 国家电投集团科学技术研究院有限公司 | Bamboo biomass poly-generation method and system |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113891852A (en) * | 2019-03-29 | 2022-01-04 | 阿玛蒂克斯控制公司 | Method for producing highly activated, monolithic reticulated biochar electrodes |
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| CN110299522A (en) * | 2019-06-26 | 2019-10-01 | 陕西科技大学 | A kind of preparation method of the biomass porous carbon nano-electrode material of high capacity sodium-ion battery Fluorin doped |
| CN110299522B (en) * | 2019-06-26 | 2021-05-25 | 陕西科技大学 | Preparation method of fluorine-doped biomass porous carbon nano electrode material for high-capacity sodium ion battery |
| CN110479226A (en) * | 2019-08-30 | 2019-11-22 | 郑州大学 | A kind of clay mineral/agricultural abandoned biomass compound sewage inorganic agent, preparation method and application |
| CN110479226B (en) * | 2019-08-30 | 2022-09-16 | 郑州大学 | Clay mineral/agriculture and forestry waste biomass composite sewage treatment agent, and preparation method and application thereof |
| CN112340730A (en) * | 2020-11-24 | 2021-02-09 | 海南大学 | Preparation method of microporous carbon-rich material based on carboxylation anchoring effect |
| CN112340730B (en) * | 2020-11-24 | 2022-03-29 | 海南大学 | Preparation method of microporous carbon-rich material based on carboxylation anchoring effect |
| CN113563011A (en) * | 2021-08-03 | 2021-10-29 | 宁波瑞能环境能源技术有限公司 | Novel building energy-saving material and preparation method thereof |
| CN116254124A (en) * | 2022-11-01 | 2023-06-13 | 国家电投集团科学技术研究院有限公司 | Bamboo biomass poly-generation method and system |
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