CN108439403A - A kind of method that low-temperature prewarming solution, raw material fine prepare biomass moulding activated carbon - Google Patents
A kind of method that low-temperature prewarming solution, raw material fine prepare biomass moulding activated carbon Download PDFInfo
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- CN108439403A CN108439403A CN201810603499.3A CN201810603499A CN108439403A CN 108439403 A CN108439403 A CN 108439403A CN 201810603499 A CN201810603499 A CN 201810603499A CN 108439403 A CN108439403 A CN 108439403A
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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
- C01B32/342—Preparation characterised by non-gaseous activating agents
- C01B32/348—Metallic compounds
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- C—CHEMISTRY; METALLURGY
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
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- C01B32/30—Active carbon
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- C01B32/342—Preparation characterised by non-gaseous activating agents
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Abstract
A kind of method that low-temperature prewarming solution, raw material fine prepare biomass moulding activated carbon.With sawdust, taking bamboo crumbs as raw material; phosphoric acid is activator; raw material is after the processing of low-temperature prewarming solution; it is crushed using pulverizer fine, raw material will be crushed and mixed with phosphoric acid solution, and carry out vacuum kneading; hardening is squeezed out again; pelletizing activates after hardening, through rinsing, filtering, screening, drying to get finished activated charcoal after activation.The method of the invention raw material low-temperature prewarming solution is conducive to hole opening, the fully penetrated convenient for phosphoric acid and recycling, reduces the ash content of activated carbon, and phosphoric acid and raw material come into full contact with effect, keep the pore structure of activated carbon more flourishing；Due to generating part tar in pre- pyrolytic process, be conducive to the intensity for improving activated carbon in forming process；After raw material fine crushes, grain size is essentially identical, and the activated carbon pore size distribution of preparation is more concentrated；During vacuum kneading, intergranular air is excluded, and intergranular combination is more closely knit, and the intensity of activated carbon improves.
Description
Technical field
The invention belongs to high-performance biomass pressed active carbon preparing technical fields, and specifically one kind is with sawdust, bamboo
Bits are raw material and the method that increase low-temperature prewarming solution, raw material fine process prepare high performance active carbon before activation.
Background technology
Pressed active carbon has larger size and a controllable shape, higher mechanical strength and bulk density, storage,
It is more convenient during transport, use, and without dust pollution, the purposes for the different industries that are content with very little, especially in Gas Phase Adsorption
Field is that Powdered Activated Carbon is irreplaceable.Traditional biomass moulding activated carbon is often prepared with phosphoric acid activation method, in preparation process
In, sawdust, i.e. with phosphoric acid solution admixture activation, does not carry out low-temperature prewarming solution and raw material ultra fine after drying, screening,
Under the conditions of not adding any binder, the activated carbon intensity of preparation it is poor (<90%), the relatively low (iodine sorption value of absorption property<
900mg/g, methylene blue adsorption value<180mg/g).
Granted patent ZL03125474.8 discloses a kind of preparation method of wooden vehicular active carbon, with cocoanut shell, apricot shell
Deng for raw material, phosphoric acid, zinc chloride etc. are activator, and raw material (40-100 mesh) is directly mixed with activator without low-temperature prewarming solution to be pinched
It closes, is activated after sizing, the pore volume of the activated carbon 1-5nm of preparation is preferable to the absorption property of butane more than 60%, but strong
Spend poor, column-shaped active carbon intensity 85%, spherical carbon intensity 60%.Granted patent CN104628000B discloses a kind of column coconut palm
After being mixed with binder, activator leaching is added with coconut shell flour (100-200 mesh) for raw material in shell activated carbon and preparation method thereof
Stain activates, and the activated carbon of high intensity, higher mesoporous rate, but adding due to binder are prepared for after extrusion forming, carbonization-activation
Enter, plugs part hole, the specific surface area of institute's preparing active carbon, total hole volume are smaller, and absorption property is poor.Granted patent
CN103058186B discloses a kind of method preparing granular activated carbon as raw material using sawdust, and using sawdust as raw material, phosphoric acid is to live
Agent, by adding co-catalyst, the activated carbon intensity of preparation has higher intensity and reference area, but pore-size distribution does not collect
In, mesoporous rate is not high, and the addition of co-catalyst increases ash of active carbon, has harmful effect to absorption property.
Although publication and document are all prepared for the activated carbon of better performances, it can not realize that the high of activated carbon is inhaled simultaneously
Attached performance, high intensity, pore-size distribution concentrate, and these be all in fields such as car carbon tank, solvent recoveries for activated carbon must not
Can be less.
Invention content
The technical issues of solution：The present invention is poor for existing phosphoric acid method biomass moulding activated carbon product absorption property, strong
The problems such as low, pore-size distribution is not concentrated is spent, one kind is provided and biomass moulding work is prepared by low-temperature prewarming solution, raw material fine
Property charcoal method, it is good to obtain absorption property under the conditions of not adding any catalyst and binder, and intensity is high, and aperture is concentrated respectively
Biomass moulding activated carbon.
Technical solution：A kind of low-temperature prewarming solution, raw material fine prepare biomass moulding activated carbon, are with sawdust or bamboo scraps
Raw material, then activator solution impregnate, vacuum kneading, then will mediate material extrusion molding hardening, pelletizing, high-temperature activation is rinsed
It is filtered dry dry screening to obtain, before activator solution dipping, raw material first carries out fine crushing again after the processing of low-temperature prewarming solution, low
The pre- pyrolysis temperature of temperature is 200-300 DEG C, grain size after fine crushes<200 purposes account for 85% or more；The biomass moulding is lived
Property charcoal ash content be less than 3%, intensity is more than 94%, and more than 1000mg/g, methylene blue adsorption value is more than iodine sorption value
240mg/g, specific surface area are more than 1500m2/ g, the pore volume less than 5nm account for 83% or more of total hole volume.
It prepares the low-temperature prewarming solution, the method that raw material fine prepares biomass moulding activated carbon, is original with sawdust
Expect, then activator solution impregnates, vacuum kneading, then will mediate material extrusion molding hardening, pelletizing, and high-temperature activation, rinsing is filtered
Dry sieve is got, and before activator solution dipping, raw material first carries out fine after the processing of low-temperature prewarming solution and crushes low temperature again
Pre- pyrolysis temperature is 200-300 DEG C, grain size after fine crushes<200 purposes account for 85% or more.
Activator solution compares 0.5-3 with raw material according to pure activator and over dry material quality：1 ratio mixing.
Vacuum kneading temperature is 100-180 DEG C, kneading time 1-5h.
It is 90-150 DEG C to be molded hardening temperature, time 2-6h.
400-550 DEG C of activation temperature, soak time 0.5-3h.
It will again be utilized after the solution recycling addition partial activation agents containing activator when rinsing.
The activator solution mass percent concentration is 30%-85%.
Activator is any in phosphoric acid, zinc chloride, potassium hydroxide.
Until the pH value of rinsing liquid is 3~6 when rinsing, then by product, at 150 DEG C, drying to constant weight.
Advantageous effect：
1, the method for the invention is easy to operate, easy to implement, has the characteristics that economic and environment-friendly, recyclable phosphoric acid solution,
Recycling.
2, raw material low-temperature prewarming solution is conducive to hole opening, the fully penetrated convenient for phosphoric acid and elution, reduces phosphoric acid
Consumption, while reducing the ash content of activated carbon, and coming into full contact with for phosphoric acid and raw material improves dipping and activation efficiency, make activity
The pore structure of charcoal is more flourishing；After raw material fine crushes, grain size is essentially identical, and the activated carbon pore size distribution of preparation more collects
In.
3, hemicellulose (225-325 DEG C of decomposition temperature) and cellulose (decomposition temperature 240-400 in raw material preheating solution preocess
DEG C) decomposed, the emplastics such as tar, oligosaccharide are generated, are conducive to the intensity for improving activated carbon in forming process；Raw material
After crushing, intergranular distance reduces, and Van der Waals force and chemical bond power increase between particle, are conducive to carrying for activated carbon intensity
Height, while during vacuum kneading, intergranular air is excluded, intergranular combination is more closely knit so that activated carbon
Intensity is obviously improved；The present invention is by low-temperature prewarming solution and raw material fine, in the item for not adding any catalyst and binder
Under part, the biomass moulding activated carbon of invention meets mesoporous pore size distribution concentration, high intensity, high absorption property simultaneously, realizes
The breakthrough of technology.
4, the made activated carbon of phosphoric acid method of the present invention is strong with adsorption capacity, desorption residual is low, pore-size distribution concentrates (aperture
Based on 5nm), the features such as ash content is low, intensity is high, can be used for car carbon tank, VOCs is administered, organic solvent recycling, gas essence
The fields such as system, catalyst carrier.
Description of the drawings
Fig. 1 is that a kind of low-temperature prewarming solution of the present invention, raw material fine prepare the technique stream of biomass moulding activated carbon
Cheng Tu.
Fig. 2 is the graph of pore diameter distribution of embodiment 1.
Specific implementation mode
Said program is described further below in conjunction with specific embodiment.It should be understood that these embodiments are for illustrating
The protection domain that the present invention is not intended to limit the present invention.
Using sawdust as raw material, phosphoric acid is activator, sawdust is sieved removal grit and dust, in 200-300 DEG C of Muffle
Constant temperature is pyrolyzed 2-5h in advance in stove, and raw material is crushed, grain size is less than after crushing after the processing of low-temperature prewarming solution using high speed disintegrator
200 purposes account for 85% or more.It is 0.5-3 that raw material, which will be crushed, according to pure phosphoric acid and material quality ratio：1 is mixed with dipping, phosphoric acid solution
A concentration of 30-85%, and vacuum kneading is carried out in 100-180 DEG C of vacuum kneader, after kneading, material will be mediated and be put into
It is squeezed out in molding machine, 2-6h is hardened in 90-150 DEG C of baking oven, hardening material shearing is less than to of 1cm after hardening to length
Grain is transferred to constant temperature in 400-550 DEG C of Muffle furnace and activates 0.5-3h.It is taken out after the completion of activation, with boiling water rinses, while recycling phosphorus
Acid solution, until rinsing liquid pH value be 3~6, filtering by product, drying to constant weight in 150 DEG C of baking ovens, after screening up at
Product activated carbon.After rinsing, the rinsing liquid containing phosphoric acid can utilize again after adding part phosphoric acid.
Preferred process conditions, the raw material low-temperature prewarming solution temperature are 230-270 DEG C.
Preferred process conditions, the raw material are crushed using micronizer, grain size after crushing<200 purposes account for 85% with
On.
Preferred process conditions, a concentration of 50%-70% of phosphoric acid solution, phosphoric acid solution and sawdust according to pure phosphoric acid with
Over dry material quality ratio is 1.5：1.
Preferred process conditions, kneading temperature are 140 DEG C, and kneading state is to vacuumize, kneading time 3h.
Preferred process conditions, in the activation procedure, activation temperature is 500 DEG C, soak time 1.5-2h.
Embodiment 1
Weigh be dried after raw material 120g, be pyrolyzed 3h in advance in 270 DEG C of Muffle furnace, after pulverizer crushes with matter
It measures the phosphoric acid solution that score is 55% and presses impregnating ratio (pure phosphoric acid and over dry material quality ratio, following embodiment are same) 1.5:1 carries out
Mixing, carries out vacuum kneading in 140 DEG C of vacuum kneader, after kneading, will mediate and expect to be put into molding machine to squeeze out,
3h is hardened in 120 DEG C of baking oven, constant temperature in 500 DEG C of Muffle furnace is transferred to and activates 2h.It is taken out after the completion of activation, extremely with boiling water rinses
PH value is 3~6, is dried to constant weight in 150 DEG C of baking ovens after filtering and gets product activated carbon.After tested：Made activated carbon-iodine is inhaled
Assignments 1128.43mg/g, methylene blue adsorption value reach 255mg/g, ash content 1.28%, intensity 96.73%, butane working capacity
15.5g/100mL, butane hold attached property 1.52g/100mL, and pore volume of the aperture less than 5nm accounts for the 84.92% of total hole volume.
Embodiment 2
Weigh be dried after raw material 120g, be pyrolyzed 3h in advance in 270 DEG C of Muffle furnace, after pulverizer crushes with matter
It measures the phosphoric acid solution that score is 55% and presses impregnating ratio (pure phosphoric acid and over dry material quality ratio, following embodiment are same) 1.5:1 carries out
Mixing, carries out vacuum kneading in 140 DEG C of vacuum kneader, after kneading, will mediate and expect to be put into molding machine to squeeze out,
3h is hardened in 120 DEG C of baking oven, constant temperature in 500 DEG C of Muffle furnace is transferred to and activates 2h.It is taken out after the completion of activation, extremely with boiling water rinses
PH value is 3~6, is dried to constant weight in 150 DEG C of baking ovens after filtering and gets product activated carbon.After tested：Made activated carbon-iodine is inhaled
Assignments 1210.25mg/g, methylene blue adsorption value reach 240mg/g, ash content 1.74%, intensity 94.73%, butane working capacity
17.9g/100mL, butane hold attached property 1.83g/100mL, and pore volume of the aperture less than 5nm accounts for the 85.27% of total hole volume.
Embodiment 3
Weigh be dried after raw material 120g, be pyrolyzed 3h in advance in 250 DEG C of Muffle furnace, after pulverizer crushes with matter
It measures the phosphoric acid solution that score is 80% and presses impregnating ratio (pure phosphoric acid and over dry material quality ratio, following embodiment are same) 1.5:1 carries out
Mixing, carries out vacuum kneading in 140 DEG C of vacuum kneader, after kneading, will mediate and expect to be put into molding machine to squeeze out,
3h is hardened in 120 DEG C of baking oven, constant temperature in 550 DEG C of Muffle furnace is transferred to and activates 1.5h.It is taken out after the completion of activation, uses boiling water rinses
It is 3~6 to pH value, is dried to constant weight in 150 DEG C of baking ovens after filtering and get product activated carbon.After tested：Made activated carbon-iodine
Adsorptive value 1163.24mg/g, methylene blue adsorption value reach 255mg/g, ash content 2.06%, intensity 96.2%, butane working capacity
16.2g/100mL, butane hold attached property 1.67g/100mL, and pore volume of the aperture less than 5nm accounts for the 84.51% of total hole volume.
Embodiment 4
Weigh be dried after raw material 120g, be pyrolyzed 3h in advance in 230 DEG C of Muffle furnace, after pulverizer crushes with matter
It measures the phosphoric acid solution that score is 55% and presses impregnating ratio (pure phosphoric acid and over dry material quality ratio, following embodiment are same) 1.5:1 carries out
Mixing, carries out vacuum kneading in 140 DEG C of vacuum kneader, after kneading, will mediate and expect to be put into molding machine to squeeze out,
3h is hardened in 120 DEG C of baking oven, constant temperature in 450 DEG C of Muffle furnace is transferred to and activates 1h.It is taken out after the completion of activation, extremely with boiling water rinses
PH value is 3~6, is dried to constant weight in 150 DEG C of baking ovens after filtering and gets product activated carbon.After tested：Made activated carbon-iodine is inhaled
Assignments 1073.25mg/g, methylene blue adsorption value reach 270mg/g, ash content 1.32%, intensity 95.47%, butane working capacity
15.8g/100mL, butane hold attached property 1.32g/100mL, and pore volume of the aperture less than 5nm accounts for the 83.64% of total hole volume.
Above example is merely illustrative of the invention's technical idea, and protection scope of the present invention cannot be limited with this, every
According to technological thought proposed by the present invention, any change done in technical solution is each fallen within the scope of the present invention；
The technology that the present invention is not directed to can be realized by the prior art.
Claims (10)
1. a kind of low-temperature prewarming solution, raw material fine prepare biomass moulding activated carbon, with sawdust or taking bamboo crumbs as raw material, then
Activator solution impregnates, vacuum kneading, then will mediate material extrusion molding hardening, pelletizing, high-temperature activation, rinsing filtration drying screening
It obtains, which is characterized in that before activator solution dipping, raw material first carries out fine crushing again after the processing of low-temperature prewarming solution,
Low-temperature prewarming solution temperature is 200-300 DEG C, grain size after fine crushes<200 purposes account for 85% or more；The biomass moulding
The ash content of activated carbon is less than 3%, and intensity is more than 94%, and iodine sorption value is more than 1000mg/g, and methylene blue adsorption value is more than
240mg/g, specific surface area are more than 1500m2/ g, the pore volume less than 5nm account for 83% or more of total hole volume.
2. low-temperature prewarming solution described in claim 1 is prepared, the method that raw material fine prepares biomass moulding activated carbon, with wood
Bits are raw material, and then activator solution impregnates, vacuum kneading, then will mediate material extrusion molding hardening, pelletizing, high-temperature activation, drift
Filtration drying is washed to sieve to obtain, which is characterized in that activator solution dipping before, raw material first through low-temperature prewarming solution processing after again into
It is 200-300 DEG C that row fine, which crushes low-temperature prewarming solution temperature, grain size after fine crushes<200 purposes account for 85% or more.
3. it is according to claim 2 prepare low-temperature prewarming solution, the method that raw material fine prepares biomass moulding activated carbon,
It is characterized in that, activator solution compares 0.5-3 with raw material according to pure activator and over dry material quality：1 ratio mixing.
4. it is according to claim 2 prepare low-temperature prewarming solution, the method that raw material fine prepares biomass moulding activated carbon,
It is characterized in that, vacuum kneading temperature is 100-180 DEG C, kneading time 1-5h.
5. it is according to claim 2 prepare low-temperature prewarming solution, the method that raw material fine prepares biomass moulding activated carbon,
It is characterized in that, molding hardening temperature is 90-150 DEG C, time 2-6h.
6. it is according to claim 2 prepare low-temperature prewarming solution, the method that raw material fine prepares biomass moulding activated carbon,
It is characterized in that, 400-550 DEG C of activation temperature, soak time 0.5-3h.
7. it is according to claim 2 prepare low-temperature prewarming solution, the method that raw material fine prepares biomass moulding activated carbon,
It is characterized in that, will again be utilized after the solution recycling addition partial activation agents containing activator when rinsing.
8. it is according to claim 2 prepare low-temperature prewarming solution, the method that raw material fine prepares biomass moulding activated carbon,
It is characterized in that, the activator solution mass percent concentration is 30%-85%.
9. it is according to claim 2 prepare low-temperature prewarming solution, the method that raw material fine prepares biomass moulding activated carbon,
It is characterized in that, activator is any in phosphoric acid, sulfuric acid, zinc chloride, potassium hydroxide.
10. it is according to claim 2 prepare low-temperature prewarming solution, raw material fine prepares the side of biomass moulding activated carbon
Method, which is characterized in that until the pH values of rinsing liquid are 3 ~ 6 when rinsing, then drying to constant weight at 150 DEG C by product.
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Cited By (8)
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| CN109292773A (en) * | 2018-10-31 | 2019-02-01 | 张俊霞 | A kind of active carbon and its preparation method and application using trees preparation |
| CN110713183A (en) * | 2019-08-15 | 2020-01-21 | 中国林业科学研究院林产化学工业研究所 | Molded granular activated carbon prepared from fast growing wood processing residues and preparation method thereof |
| CN110790275A (en) * | 2019-11-25 | 2020-02-14 | 中国林业科学研究院林产化学工业研究所 | Method for improving strength of formed activated carbon by matching biomass raw materials and product thereof |
| CN112429732A (en) * | 2020-12-02 | 2021-03-02 | 中国林业科学研究院林产化学工业研究所 | Lignin-based formed activated carbon and preparation method thereof |
| CN113200543A (en) * | 2021-06-18 | 2021-08-03 | 南京林业大学 | Method for preparing activated carbon precursor by intervention of biomass oil |
| CN113213477A (en) * | 2021-06-09 | 2021-08-06 | 中国林业科学研究院林产化学工业研究所 | Preparation method of straw activated carbon with high adsorption performance |
| CN113753891A (en) * | 2021-09-23 | 2021-12-07 | 福建省鑫森炭业股份有限公司 | Wooden activated carbon for vehicle carbon tank and preparation technology |
| CN113912058A (en) * | 2021-10-15 | 2022-01-11 | 青岛华世洁环保科技有限公司 | Preparation method of honeycomb activated carbon |
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| CN110713183A (en) * | 2019-08-15 | 2020-01-21 | 中国林业科学研究院林产化学工业研究所 | Molded granular activated carbon prepared from fast growing wood processing residues and preparation method thereof |
| CN110790275A (en) * | 2019-11-25 | 2020-02-14 | 中国林业科学研究院林产化学工业研究所 | Method for improving strength of formed activated carbon by matching biomass raw materials and product thereof |
| CN112429732A (en) * | 2020-12-02 | 2021-03-02 | 中国林业科学研究院林产化学工业研究所 | Lignin-based formed activated carbon and preparation method thereof |
| CN113213477A (en) * | 2021-06-09 | 2021-08-06 | 中国林业科学研究院林产化学工业研究所 | Preparation method of straw activated carbon with high adsorption performance |
| CN113200543A (en) * | 2021-06-18 | 2021-08-03 | 南京林业大学 | Method for preparing activated carbon precursor by intervention of biomass oil |
| CN113753891A (en) * | 2021-09-23 | 2021-12-07 | 福建省鑫森炭业股份有限公司 | Wooden activated carbon for vehicle carbon tank and preparation technology |
| CN113912058A (en) * | 2021-10-15 | 2022-01-11 | 青岛华世洁环保科技有限公司 | Preparation method of honeycomb activated carbon |
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