CN105174259B - A kind of preparation can be in the pressed active carbon method of water float - Google Patents
A kind of preparation can be in the pressed active carbon method of water float Download PDFInfo
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- CN105174259B CN105174259B CN201510576281.XA CN201510576281A CN105174259B CN 105174259 B CN105174259 B CN 105174259B CN 201510576281 A CN201510576281 A CN 201510576281A CN 105174259 B CN105174259 B CN 105174259B
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- active carbon
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Abstract
The present invention relates to a kind of preparation can be in the pressed active carbon method of water float.Its technical scheme is: joined by powdery sodium salt by the phosphoric acid lignocellulose-like biomass of low-temperature heat, after stirring, carry out extruded, dry, charcoal activates, wash, be dried, thus has obtained the pressed active carbon that may float in water；Described powdery sodium salt is the sodium chloride of powder, sodium sulfate or tertiary sodium phosphate；Providing the benefit that: 1) pressed active carbon for preparing of the present invention can float in water on 36h continuously；2) gained pressed active carbon will not ftracture in flotation process, will not fall bits, will not deform, and specific surface area is 400 ~ 1500m2/g；3), during extrusion forming, briquetting pressure is easily stable in the range of specified pressure ± 0.2MPa；4) material is difficult to adhesion mold wall, and demoulding posterior synechiae is in the quality of material of mold wall, and less than in demoulding front mold the 0.1% of quality of material, mould removal is easy.
Description
Technical field
The present invention relates to technical field of active carbon, can be in the pressed active carbon side of water float particularly to a kind of preparation
Method.
Background technology
Pressed active carbon has the advantages such as geometric shape rule, density is big, unit volume adsorbance is high, mechanical strength is good,
Can be widely used for the numerous areas such as gas absorption, sewage disposal, energy storage.Prepare pressed active carbon, can use and be extruded into
Type method.Before extrusion molding, binding agent can be added, it is possible to be not added with binding agent.Wherein, being not added with adhesive method, preparation technology is relatively
For simply.Research shows, with lignocellulose-like biomass as raw material, and H3PO4For activator, can be in the feelings without added binding agents
Pressed active carbon is prepared under condition.In recent years, such preparation method is by more concern.
Such as, and Lou Xuchun (chemical method prepares the research of wooden pressed active carbon, master thesis, and 2012, Nanjing forestry
University) etc. phosphoric acid is added cedar sawdust, prepared specific surface area through steps such as plasticizing, molding, charcoal activation and reached 1770 m2The one-tenth of/g
Type activated carbon.Li great Wei etc. (Li great Wei, Tang Ruiyuan, Tian Yuanyu etc., Bioresources, 2014,9(1), 1246-1254) with
Poplar bits are raw material, H3PO4For activator, through steps such as plasticizing, molding, in the case of without added binding agents, prepare and compared table
Area is the pressed active carbon of 951 m2/g.Jiang should wait (patent publication No.: CN103922338A) to disclose one with bamboo bits by ladder
Deng for raw material, phosphoric acid is activator, the method preparing granular active carbon.Wang Zhigao (Wang Zhigao, Jiang Jianchun, Deng Xianlun, forest products
Learn with industry, 2005,25(2), 39-42) etc. with wood flour as raw material, phosphoric acid is activator, use kneader to wood flour phosphoric acid mix
Close material and carry out pretreatment, prepare decolouring granular active carbon.Diana P. Vargas etc. (Diana P. Vargas,
Giraldo, L., Silvestre-Albero, J. etc., Adsorption-Journal of the International
Adsorption Society, 2011,17(3), 497-504) and with coconut husk as raw material, H3PO4For activator, prepare specific surface
Amass and reach 1331 m2The sheet shaped activated carbon of/g.Afterwards, this seminar (Vargas, D. P., Giraldo, L., Moreno-
Pirajan, J. C., International Journal of Molecular Sciences, 2012,13(7), 8388-
8397) utilize again palm shell and phosphoric acid, in the case of without added binding agents, prepare CO2Absorption pressed active carbon.
Above-mentioned report, provides good thinking for preparing pressed active carbon with lignocellulose-like biomass.But still deposit
In following shortcoming: 1) carry phosphoric acid wood flour or bamboo and consider to be worth doing after heat treatment, there is higher viscosity, also there is after pressurization mobility, make
Obtain material to be difficult at specified pressure compacted under, and be easily adhered at mould wall or enter in die gap, so that the demoulding is stranded
Difficulty, even destroys body；2) gained pressed active carbon is difficult to swim in water for a long time, is not suitable for needing floating occasion.
Such as, after the pollutant such as oils enter the water bodys such as river, river, lake, the water surface can be swum in, use and can give by floating pressed active carbon
Raising and the recovery of activated carbon with absorption, beneficially adsorption efficiency.
Summary of the invention
The purpose of the present invention is aiming at the drawbacks described above that prior art exists, it is provided that a kind of preparation can be at water float
Pressed active carbon method, uses the method, the molding under a steady pressure of phosphoric acid material, material can be difficult to adhesion mould
Wall, the demoulding is easy, and body is regular, and gained pressed active carbon can swim in water for a long time, and specific surface area is 400-1500
m2/g。
Its technical scheme is: joined by powdery sodium salt by the phosphoric acid lignocellulose-like biomass of low-temperature heat,
After stirring, carry out extruded, dry, charcoal activates, wash, be dried, thus has obtained the movable forming that may float in water
Property charcoal；
Described powdery sodium salt is the sodium chloride of powder, sodium sulfate or tertiary sodium phosphate, and particle diameter is 18 ~ 150 μm, addition
For lignocellulose-like biomass butt quality used 0.1 ~ 1.2 times；
Described lignocellulose-like biomass, refers to wood flour, Pericarppium arachidis hypogaeae, cotton stem or straw, and particle diameter is 0.1-3.0
mm；
Described phosphoric acid lignocellulose-like biomass, is by being the phosphate aqueous solution of 20 ~ 65wt% by concentration, with
Lignocellulose-like biomass is mixed to get；In this phosphoric acid lignocellulose-like biomass, phosphoric acid presses pure H3PO4Meter, with dry
The mass ratio of base lignocellulose-like biomass is 0.1-2.0；
Low-temperature heat, refers to by phosphoric acid lignocellulose-like biomass at 60 ~ 100 DEG C, blast heating 40-120
min。
Above-mentioned extruded during, briquetting pressure can be stablized at 2-40MPa, dwell time >=30s.
Above-mentioned is dried, and is all in air dry oven, in 90 ~ 120 DEG C of forced air drying 0.5 ~ 18h.
Above-mentioned charcoal activation, refers to, by material under the protection of noble gas, with the heating rate of 1 ~ 80 DEG C/min, add
Heat is to 400 ~ 700 DEG C, and keeps 0.5 ~ 2h.
Above-mentioned washing, refers to molded body cyclic washing with deionized water or distilled water, until washing liquid pH value is 6 ~ 7.
Compared with prior art, it provides the benefit that the present invention: pressed active carbon that 1) present invention prepares can continuously 36h it
On float in distilled water, tap water, lake water or sea water；2) gained pressed active carbon will not ftracture in flotation process, will not
Falling bits, will not deform, specific surface area is 400 ~ 1500 m2/g；3), during extrusion forming, briquetting pressure is easily stable is specifying
In the range of pressure ± 0.2MPa；4) material is difficult to adhesion mold wall, and demoulding posterior synechiae is in the quality of material of mold wall, less than de-
In mould front mold the 0.1% of quality of material, mould removal is easy.
Detailed description of the invention
Below in conjunction with example, the invention will be further described, but is not used in the restriction present invention.
Embodiment 1
Being joined by the phosphoric acid that concentration is 40wt% in the dry poplar bits that particle diameter is 0.1 ~ 0.9mm, addition is poplar bits
1.1 times of quality (by pure H3PO4Meter).Thereafter, they are placed in air dry oven, heat 75min at 80 DEG C.Adding particle diameter is
The powdery sodium chloride of 100 ~ 150 μm, addition is 1.2 times of wood flour butt quality used, then is stirred continuously, until visually
Mix homogeneously.Then, material is placed in mould, is slowly pressurized to 13MPa and keeps 1min.By gained molded body at N2Protection
Under, it is heated to 600 DEG C with the heating rate of 10 DEG C/min, and keeps 1h.With deionized water cyclic washing molded body, until washing liquid
PH value be 6.Finally, by molded body at 110 DEG C of blast heating 10h, i.e. can get pressed active carbon.Gained pressed active carbon energy
Enough swimming in tap water, specific surface area is 870m2/ g, total pore volume is 0.51ml/g, and productivity is 46%；Pressure in preparation process
Can stablize at 13 ± 0.2 Mpa.
Embodiment 2
The phosphoric acid that concentration is 50wt% joins the dry cotton stalk powder that particle diameter is 0.1 ~ 1.0 mm, and addition is cotton stalk powder
1.0 times of quality (by pure H3PO4Meter).Thereafter, they are placed in air dry oven, heat 120min at 60 DEG C.Adding particle diameter is
The powdered acid sodium of 100 ~ 150 μm, addition is 0.1 times of cotton stalk powder butt quality used, is stirred continuously, until visually
Mix homogeneously.Then, material is placed in mould, is slowly pressurized to 8MPa and keeps 1min.By gained molded body at N2Under protection,
It is heated to 560 DEG C with the heating rate of 8 DEG C/min, and keeps 1h.With deionized water cyclic washing molded body, until the pH of washing liquid
It is 6.6.Finally, by molded body at 110 DEG C of blast heating 12h, i.e. can get pressed active carbon.Gained pressed active carbon can float
Floating in deionized water, specific surface area is 810m2/ g, total pore volume is 0.48ml/g, and productivity is 45%；In preparation process, pressure can
Stable at 8 ± 0.2 Mpa.
Embodiment 3
The phosphoric acid that concentration is 55wt% joins the drying peanut shell powder that particle diameter is 0.2 ~ 1.0 mm, and addition is Semen arachidis hypogaeae
0.1 times of shell opaque amount (by pure H3PO4Meter).Thereafter, they are placed in air dry oven, heat 40min at 100 DEG C.Add grain
Footpath is the powdered acid trisodium of 18 ~ 150 μm, and addition is 0.9 times of peanut hull meal butt quality used, is stirred continuously, until
Visually mix homogeneously.Then, by material as mould, slowly it is pressurized to 6MPa and keeps 1min.By gained molded body at N2
Under protection, it is heated to 540 DEG C with the heating rate of 5 DEG C/min, and keeps 1h.With deionized water cyclic washing molded body, until
The pH of washing liquid is 6.3.Finally, by molded body at 110 DEG C of blast heating 13h, i.e. can get pressed active carbon.Gained Constitutive active
Charcoal can floating in deionized water, specific surface area is 950m2/ g, total pore volume is 0.61ml/g, and productivity is 52%；Preparation process
Middle pressure can be stablized at 6 ± 0.1 Mpa.
Embodiment 4
The phosphoric acid that concentration is 35wt% joins the dry straw powder that particle diameter is 0.2 ~ 1.0 mm, and addition is straw powder
2 times of quality (by pure H3PO4Meter).Thereafter, they are placed in air dry oven, heat 65min at 85 DEG C.Add particle diameter be 89 ~
The powdery sodium sulfate of 150 μm, addition is 1.1 times of straw dried bean noodles substrate amount used, then is stirred continuously, until visually mixing
Close uniformly.Then, material is placed in mould, is slowly pressurized to 40MPa, dwell time 30s.By gained molded body at N2Protection
Under, with the heating rate of 80 DEG C/min, it is heated to 700 DEG C, and keeps 0.5h.With deionized water cyclic washing molded body, until
The pH of washing liquid is 7.Finally, by molded body at 120 DEG C of forced air drying 0.5h, i.e. can get pressed active carbon.Gained Constitutive active
Charcoal can swim in tap water, and specific surface area is 1100m2/ g, total pore volume is 0.70ml/g, and productivity is 43%；In preparation process
Pressure can be stablized at 40 ± 0.1 Mpa.
The above, be only the part preferred embodiment of the present invention, and any those of ordinary skill in the art all may profit
Revised or be revised as the technical scheme of equivalent by the technical scheme of above-mentioned elaboration.Therefore, according to the technology of the present invention
Any simple modification that scheme is carried out or substitute equivalents, belong to the greatest extent the scope of protection of present invention.
Claims (5)
1. prepare and can it is characterized in that in a pressed active carbon method for water float: powdery sodium salt is joined and is added by low temperature
The phosphoric acid lignocellulose-like biomass that heat is crossed, after stirring, carry out extruded, dry, charcoal activates, wash, dry,
Thus obtained the pressed active carbon that may float in water；
Described powdery sodium salt is the sodium chloride of powder, sodium sulfate or tertiary sodium phosphate, and particle diameter is 18 ~ 150 μm, and addition is institute
By lignocellulose-like biomass butt quality 0.1 ~ 1.2 times；
Described lignocellulose-like biomass, refers to wood flour, Pericarppium arachidis hypogaeae, cotton stem or straw, and particle diameter is 0.1-3.0 mm；
Described phosphoric acid lignocellulose-like biomass, is by being the phosphate aqueous solution of 20 ~ 65wt% by concentration, with wooden
Cellulose series biomass is mixed to get；In this phosphoric acid lignocellulose-like biomass, phosphoric acid presses pure H3PO4Meter, with butt wood
The mass ratio of matter cellulose series biomass is 0.1-2.0；
Low-temperature heat, refers to by phosphoric acid lignocellulose-like biomass at 60 ~ 100 DEG C, blast heating 40-120 min.
A kind of preparation the most according to claim 1 can is characterized in that: described in the pressed active carbon method of water float
During extruded, briquetting pressure can be stablized at 2-40MPa, dwell time >=30s.
A kind of preparation the most according to claim 1 can is characterized in that: described in the pressed active carbon method of water float
It is dried, is all in air dry oven, in 90 ~ 120 DEG C of forced air drying 0.5 ~ 18h.
A kind of preparation the most according to claim 1 can is characterized in that: described in the pressed active carbon method of water float
Charcoal activates, and refers to by material under the protection of noble gas, with the heating rate of 1 ~ 80 DEG C/min, is heated to 400 ~ 700 DEG C,
And keep 0.5 ~ 2h.
A kind of preparation the most according to claim 1 can is characterized in that: described in the pressed active carbon method of water float
Washing, refers to pressed active carbon cyclic washing with deionized water or distilled water, until washing liquid pH value is 6 ~ 7.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11349319A (en) * | 1998-06-04 | 1999-12-21 | Mitsubishi Chemical Corp | Production of activated carbon |
| JPH11349320A (en) * | 1998-06-04 | 1999-12-21 | Mitsubishi Chemical Corp | Production of activated carbon |
| CN101121516A (en) * | 2007-08-07 | 2008-02-13 | 江西省绿野木业有限公司 | Multifunctional active carbon |
| CN103058186A (en) * | 2012-03-26 | 2013-04-24 | 玉山县三清活性炭有限公司 | Method of preparing sawdust as raw material into particular active carbons |
| CN103771409A (en) * | 2012-10-23 | 2014-05-07 | 天津德为环保工程设备有限公司 | Preparation method for molded biomass active carbon with crop straw as raw material |
-
2015
- 2015-09-11 CN CN201510576281.XA patent/CN105174259B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11349319A (en) * | 1998-06-04 | 1999-12-21 | Mitsubishi Chemical Corp | Production of activated carbon |
| JPH11349320A (en) * | 1998-06-04 | 1999-12-21 | Mitsubishi Chemical Corp | Production of activated carbon |
| CN101121516A (en) * | 2007-08-07 | 2008-02-13 | 江西省绿野木业有限公司 | Multifunctional active carbon |
| CN103058186A (en) * | 2012-03-26 | 2013-04-24 | 玉山县三清活性炭有限公司 | Method of preparing sawdust as raw material into particular active carbons |
| CN103771409A (en) * | 2012-10-23 | 2014-05-07 | 天津德为环保工程设备有限公司 | Preparation method for molded biomass active carbon with crop straw as raw material |
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