CN105129797B - A kind of preparation method of ammonification-activation plant activated carbon - Google Patents
A kind of preparation method of ammonification-activation plant activated carbon Download PDFInfo
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- CN105129797B CN105129797B CN201510428036.4A CN201510428036A CN105129797B CN 105129797 B CN105129797 B CN 105129797B CN 201510428036 A CN201510428036 A CN 201510428036A CN 105129797 B CN105129797 B CN 105129797B
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Abstract
The invention discloses a kind of preparation method of ammonification-activation plant activated carbon, comprise the following steps：（1）Ammoniated treatment is carried out to phyteral raw material using aminating agents such as urea, ammonium hydrogen carbonate, ammoniacal liquor, the raw material after ammonification is obtained；（2）By step（1）In ammonification after raw material and activator mix, impregnate 2 ~ 12h, the raw material after the ammonification is 1 with the mass ratio of activator：0.5~2.0；（3）Raw material after dipping is 300~800o30~60min of carbonization-activation under C, obtains activated carbon；（4）By washing active carbon, drying, product is obtained final product.Preparation method low production cost of the invention, simple production process, obtained activated carbon has high specific surface area and more rich functional group relative to conventional method.
Description
Technical field
The invention belongs to field of functional materials, the preparation side of more particularly to a kind of ammonification-activation plant activated carbon
Method.
Background technology
Activated carbon as a kind of common adsorbent, be widely used in harmful substance in gas phase and liquid phase absorption and
Removal.The ability of its absorption polluter is mostly derived from the aperture structure and abundant functional group (carboxyl, lactone group, phenol of prosperity
The acidic functionalities such as hydroxyl and basic functionality).In recent years, in order to meet the continuous market demand for expanding and consumer to higher
The requirement of activated carbon is imitated, the producer improves its physicochemical properties and absorption property usually through the method such as modified.Many researchs
Prove, plant activated carbon has the advantages that quality is high, performance is good.So, phyteral raw material is obtained in activated carbon preparation field
Substantial amounts of popularization, application.In plant activated carbon traditional preparation methods, directly soaked after charcoal precursor is crushed
Stain, activation, cause activator to impregnate insufficient, and utilization rate is low, and dip time is long, and activation temperature is high, activated carbon specific surface area
It is low, the defect such as number of functional groups is few.For the deficiency that conventional method is present, propose the preparation side of phyteral raw material ammoniated treatment
Method.
Through retrieval, the technique that ammonification-activation method prepares plant activated carbon is currently a technological gap.
The content of the invention
The present invention overcomes conventional method to prepare the weak point of activated carbon, there is provided a kind of ammonification-activation plant activated carbon
Process.Phyteral raw material is first carried out ammoniated treatment by the method during activated carbon is prepared, and then carries out charing work
Change.Activated carbon prepared by the method has the surface functional group of specific surface area higher and prosperity.
Technical scheme is as follows：
A kind of preparation method of ammonification-activation plant activated carbon, comprises the following steps：
(1) ammoniated treatment is carried out to phyteral raw material using aminating agents such as urea, ammonium hydrogen carbonate or ammoniacal liquor, obtains ammonification
Raw material afterwards；
(2) raw material after ammonification in step (1) and activator are mixed, 2~12h, the ammonification is impregnated at 20~30 DEG C
Raw material afterwards is 1 with the mass ratio of activator：0.5~2.0；
(3) 30~60min of carbonization-activation at 300~800 DEG C of the raw material after dipping, obtains activated carbon；
(4) by washing active carbon, drying, product is obtained final product.
Before phyteral raw material carries out ammoniated treatment, phyteral raw material is pre-processed, preprocess method is：By plant
Matter raw material is washed, dried, being crushed to 20~40 mesh；The benefit for being pre-processed is：In order that the process of ammoniated treatment is more filled
Point, aminating agent is bigger with phyteral raw material reaction contact area, to reduce the ammonification time, improves efficiency.
In step (1), described phyteral raw material is one or more mixing of reed, giantreed or great Ye reeds, by examination
Checking, above-mentioned three kinds are planted raw material of substance reed, giantreed or great Ye reeds using effect after ammonification-activation process preferably, with compared with
Specific surface area high and the functional group of prosperity.
In step (1), when aminating agent is urea or ammonium hydrogen carbonate, the specific method of ammoniated treatment is：By phyteral
Raw material is 0.03~0.08 according to urea or ammonium hydrogen carbonate and the mass ratio of phyteral raw material：1 mixes with urea or ammonium hydrogen carbonate,
It is dissolved in water, seals, 1~6h is kept at 90~100 DEG C, preferable temperature is 100 DEG C.
By experimental demonstration and analysis, obtain the mass ratio of urea or ammonium hydrogen carbonate and phyteral raw material for 0.03~
0.08：When 1, the effect and efficiency of ammonification are all best, when ratio is higher, not only waste aminating agent, pollution environment, and
Trouble is will also result in during subsequent wash；When ratio is relatively low, ammoniation is not embodied sufficiently, activated carbon do not obtain compared with
Specific surface area high and the functional group of prosperity.
In step (1), when aminating agent is ammoniacal liquor, the specific method of ammoniated treatment is：By phyteral raw material according to ammonia
Water is 0.01~0.05 with the mass ratio of phyteral raw material：1 is well mixed with ammoniacal liquor, sealing, and 5~14d is kept at 18~30 DEG C,
Preferable temperature is 25 DEG C.Preferably, the mass concentration of ammoniacal liquor is 3~15%.
By experimental demonstration and analysis, it is 0.01~0.05 to obtain ammoniacal liquor with the mass ratio of phyteral raw material：When 1, ammonification
Effect and efficiency be all best, when ratio is higher, aminating agent, pollution environment are not only wasted, and during subsequent wash
Trouble can be caused；When ratio is relatively low, ammoniation is not embodied sufficiently, and activated carbon does not obtain specific surface area higher
With flourishing functional group.
In step (2), activator is phosphoric acid solution or potassium hydroxide, the mass fraction of the phosphoric acid solution for 30~
55%.
In step (2), it is preferred that the dip time is 2~8h.
Situation according to the phyteral raw material after ammonification impregnates 2~8h, and this dip time can make the phyteral after ammonification former
Material fully activation, if the time is too short, dipping is incomplete, and dipping effect is undesirable；If overlong time, lose time, reduce
Efficiency.
In step (3), it is preferred that the temperature is 300~450 DEG C, the time is 30~60min.At ammonification
After reason, can significantly reduce carburizing temperature and time (carburizing temperature of the phyteral method for preparation of active carbon of non-ammonification is 500~
900 DEG C, carbonization time be 1~4h), experiment proves that the carburizing temperature and time disclosure satisfy that the mark of the phosphorus content of activated carbon
It is accurate.
In step (4), washing active carbon to pH stable is dried again 7.0 or so, reason is：Washing active carbon
To acid or alkalescence, the reaction of activated carbon environment may be influenceed, such as if washing active carbon to alkalescence, then
May be reacted with the acidic materials in activated carbon environment.
Ammonification makes cellulose for phyteral raw material, the chemical bonds that can be destroyed between lignin and polysaccharide, and half is fine
Dimension element and lignin separation, more readily soluble hydroxyl lignin is changed into by insoluble lignin, and avicel cellulose becomes amorphous fibre
Dimension element, causes cell expansion so that phyteral raw material mix becomes loose；Also, it is thick in phyteral raw material in ammonifying process
The content of albumen is significantly improved, it is possible to increase amido functional group quantity.During prepared by plant activated carbon, by phyteral
Raw material carries out ammoniated treatment, can effectively strengthen dipping effect, improves the specific surface area of activated carbon, increases activated carbon functional group
Quantity.
It is of the invention to be had the advantage that compared with traditional preparation method：
(1) raw material uses the phyteral raw materials such as stalk, with widely distributed, with low cost advantage.
(2) aminating agent consumption is small, and pollution on the environment is small.
(3) due to ammoniation, activator usage amount is reduced, and activation temperature reduction, cost-effective, reducing energy consumption is reduced
Pollution.
(4) low production cost, simple production process, obtained activated carbon has compared with high-ratio surface relative to conventional method
Product and more rich functional group.
(5) by many experiments and analysis, the adsorption effect of activated carbon in water that preparation method of the invention is obtained is than common side
The adsorption effect of the activated carbon that method is prepared is more preferable.
Specific embodiment
With reference to embodiment, the present invention is further described.
Embodiment 1
Reed is washed, is dried, being crushed to 40 mesh；Injection is equivalent to the ammonia that reed dry matter weight mass concentration is 3%
Water is mixed with it, sealing, keeps 7d to carry out ammoniated treatment at 25 DEG C；Reed powder and 45wt.% phosphoric acid after ammonification is molten
Liquid in mass ratio 1:1 room temperature immersion 5h；Dipping thing is transferred to crucible and is built in Muffle furnace, carbonization-activation 40min at 300 DEG C, from
So it is cooled to room temperature；It is 7 or so, separation of solid and liquid, drying that gained activated carbon is washed with deionized to pH.Gained activated carbon compared with
Activated carbon specific surface area prepared by conventional method reference examples 1 improves 20%, and total number of functional groups improves 46%.
Reference examples 1
Reed washed, is dried, being crushed to 40 mesh, by reed powder and 45wt.% phosphoric acid solutions in mass ratio 1:2 dippings
10h；Dipping thing is transferred to crucible and is built in Muffle furnace, and carbonization-activation 60min, naturally cools to room temperature at 500 DEG C；Gained is lived
Property charcoal be washed with deionized to pH be 7 or so, separation of solid and liquid, drying.
Embodiment 2
Reed is washed, is dried, being crushed to 40 mesh；The urea equivalent to reed dry matter weight 7% is taken, per 10g reeds
Dry matter weight adds 2ml water dissolves, and aqueous solution of urea is mixed with reed powder, and sealing keeps 2h at 100 DEG C, carries out ammonification
Treatment；By the reed powder after ammonification and potassium hydroxide in mass ratio 1:2 impregnate 2h at 30 DEG C；It is built-in that dipping thing is transferred to nickel crucible
In Muffle furnace, carbonization-activation 60min, naturally cools to room temperature at 650 DEG C；Gained activated carbon is washed with deionized to pH
It is 7 or so, separation of solid and liquid, drying.Its specific surface area improves 15% compared with conventional method reference examples 2, and surface functional group quantity is improved
50%.
Reference examples 2
Reed washed, is dried, being crushed to 40 mesh, by reed powder and potassium hydroxide in mass ratio 1:2 dipping 8h；Dipping
Thing is transferred to crucible and is built in Muffle furnace, and carbonization-activation 120min, naturally cools to room temperature at 900 DEG C；Gained activated carbon is used
It is 7 or so, separation of solid and liquid, drying that deionized water is washed to pH.
Embodiment 3
Reed is washed, is dried, being crushed to 40 mesh；The ammonium hydrogen carbonate of reed powder dry matter weight 5% is taken, per 10g reeds
Reed powder dry matter weight adds 2ml water dissolves, and ammonium bicarbonate aqueous solution is mixed with reed powder, and sealing keeps at 100 DEG C
4h, carries out ammoniated treatment；By reed powder after ammonification and 45wt.% phosphoric acid solutions in mass ratio 1:1.5 impregnate 8h at 20 DEG C；Leaching
Stain thing is transferred to crucible and is built in Muffle furnace, and carbonization-activation 60min, naturally cools to room temperature at 400 DEG C；Gained activated carbon is used
It is 7 or so, separation of solid and liquid, drying that deionized water is washed to pH.Its specific surface area improves 15% compared with conventional method reference examples 3,
Number of functional groups improves 18%.
Reference examples 3
Reed washed, is dried, being crushed to 40 mesh, by reed powder and 45wt.% phosphoric acid solutions in mass ratio 1:1.5 leachings
Stain 8h；Dipping thing is transferred to crucible and is built in Muffle furnace, and carbonization-activation 90min, naturally cools to room temperature at 650 DEG C；By gained
It is 7 or so, separation of solid and liquid, drying that activated carbon is washed with deionized to pH.
Table 1：Activated carbon specific surface area, aperture parameters and number of functional groups.
Through experiment, giantreed, great Ye reeds obtain same good effect.
Embodiment 4
Using embodiment 1 and activated carbon application obtained in comparative example 1 is in sanitary sewage, wastewater from chemical industry and pharmacy waste water,
Three kinds of sewage are shown in Table 2 by the experimental result before and after charcoal absorption.
The adsorption effect of activated carbon in water of the embodiment 1 of table 2 and comparative example 1
Residual organic matter in waste water, residual suspension etc. realize pollutant and water body by the filtering of activated carbon, absorption
Separation, table 2 can intuitively find out that the adsorption effect of the activated carbon prepared using the method for embodiment 1 is substantially better than contrast
The adsorption effect of the activated carbon of example 1.
Claims (8)
1. the preparation method of a kind of ammonification-activation plant activated carbon, it is characterized in that, comprise the following steps：
（1）Ammoniated treatment is carried out to phyteral raw material using urea, ammonium hydrogen carbonate or ammoniacal liquor aminating agent, the original after ammonification is obtained
Material；
When aminating agent is urea or ammonium hydrogen carbonate, the specific method of ammoniated treatment is：By phyteral raw material according to urea or
Ammonium hydrogen carbonate is 0.03 ~ 0.08 with the mass ratio of phyteral raw material：1 mixes with urea or ammonium hydrogen carbonate, is dissolved in water, sealing,
90 ~ 100oC keeps 1 ~ 6h；
When aminating agent is ammoniacal liquor, the specific method of ammoniated treatment is：By phyteral raw material according to ammoniacal liquor and phyteral raw material
Mass ratio be 0.01 ~ 0.05：1 is well mixed with ammoniacal liquor, sealing, 18 ~ 30oC keeps 5 ~ 14d；
（2）By step（1）In ammonification after raw material and activator mix, 20 ~ 30oC impregnates 2 ~ 12h, the original after the ammonification
Material is 1 with the mass ratio of activator：0.5~2.0；
（3）Raw material after dipping is 300~800o30~60min of carbonization-activation under C, obtains activated carbon；
（4）By washing active carbon, drying, product is obtained final product.
2. preparation method as claimed in claim 1, it is characterized in that：Before phyteral raw material carries out ammoniated treatment, to phyteral
Raw material is pre-processed, and preprocess method is：Phyteral raw material is washed, dry, crushed, be crushed to 20 ~ 40 mesh.
3. preparation method as claimed in claim 1, it is characterized in that：Step（1）In, described phyteral raw material is reed, reed
Bamboo or one or more mixing of great Ye reeds.
4. preparation method as claimed in claim 1, it is characterized in that：The mass concentration of the ammoniacal liquor is 3 ~ 15%.
5. preparation method as claimed in claim 1, it is characterized in that：Step（2）In, activator is phosphoric acid solution or hydroxide
Potassium.
6. preparation method as claimed in claim 1, it is characterized in that：Step（2）In, the dip time is 2 ~ 8h.
7. preparation method as claimed in claim 1, it is characterized in that：Step（3）In, the temperature is 350~450oC, when described
Between be 40~60min.
8. preparation method as claimed in claim 1, it is characterized in that：Step（4）In, washing active carbon to pH stable is existed
7.0 or so are dried again.
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| JP6928620B2 (en) * | 2016-05-30 | 2021-09-01 | アドベン インダストリーズ, インコーポレイテッドAdven Industries, Inc. | Activated carbon with high surface area and its manufacturing method |
| CN106219539A (en) * | 2016-07-25 | 2016-12-14 | 句容市百诚活性炭有限公司 | A kind of preparation method of high-specific surface area hierarchical porous structure activated carbon |
| CN106927461A (en) * | 2017-03-28 | 2017-07-07 | 南平元力活性炭有限公司 | A kind of high-capacity and long-life activated carbon for super capacitors production technology |
| CN107010624B (en) * | 2017-04-24 | 2019-12-03 | 安徽大学 | A kind of nitrogen for electrode of super capacitor, boron doping porous charcoal and preparation method thereof |
| CN107128918A (en) * | 2017-05-26 | 2017-09-05 | 桂林电子科技大学 | A kind of preparation and its application of N doping porous active Carbon Materials |
| CN108467036B (en) * | 2018-05-22 | 2021-10-15 | 吉林化工学院 | Desiliconized rice hull-based activated carbon and preparation method and application thereof |
| CN108821282B (en) * | 2018-08-24 | 2020-08-25 | 山东大学 | Method for preparing active carbon with high nitrogen-containing functional groups by using shrimp bran modified Cyperaceae plant-based active carbon |
| CN110156007B (en) * | 2019-06-20 | 2022-03-25 | 运城学院 | Preparation method of arundo donax linn activated carbon |
| CN110541016A (en) * | 2019-09-10 | 2019-12-06 | 贵州好菇粮农业科技有限公司 | Extraction and purification method of lentinan |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101121514A (en) * | 2007-07-27 | 2008-02-13 | 邹炎 | Water purification active carbon prepared from vegetal castoff and preparation method thereof |
| CN104445141A (en) * | 2014-11-07 | 2015-03-25 | 同济大学 | Nitrogen-doped modified porous carbon with high specific surface area and preparation method thereof |
| CN104495837A (en) * | 2014-12-04 | 2015-04-08 | 浙江大学 | Sargassum-based activated carbon and preparation method and application thereof |
-
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- 2015-07-20 CN CN201510428036.4A patent/CN105129797B/en active Active
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101121514A (en) * | 2007-07-27 | 2008-02-13 | 邹炎 | Water purification active carbon prepared from vegetal castoff and preparation method thereof |
| CN104445141A (en) * | 2014-11-07 | 2015-03-25 | 同济大学 | Nitrogen-doped modified porous carbon with high specific surface area and preparation method thereof |
| CN104495837A (en) * | 2014-12-04 | 2015-04-08 | 浙江大学 | Sargassum-based activated carbon and preparation method and application thereof |
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