CN106219545A - A kind of preparation method of sucrose base grading-hole activated carbon - Google Patents
A kind of preparation method of sucrose base grading-hole activated carbon Download PDFInfo
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- CN106219545A CN106219545A CN201610590561.0A CN201610590561A CN106219545A CN 106219545 A CN106219545 A CN 106219545A CN 201610590561 A CN201610590561 A CN 201610590561A CN 106219545 A CN106219545 A CN 106219545A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/14—Pore volume
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
- C01P2006/17—Pore diameter distribution
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Abstract
The present invention relates to the preparation method of a kind of sucrose base grading-hole activated carbon, the present invention is with sucrose as raw material, after sucrose and nickel nitrate are dissolved in water by certain mass ratio, and heated and stirred mix homogeneously, again mixed material is carried out carbonization process, after the material after carbonization is removed nickel with hydrochloric acid, washing and drying, again further for material chemical activation is processed, obtain grading-hole activated carbon.The activated carbon that the present invention prepares has hierarchical porous structure, and its intermediary hole rate reaches 37 more than 52%, and microporosity 40 57%, big porosity is 6 9%；The activated carbon that the present invention prepares simultaneously has high-specific surface area, and specific surface area is up to 1214 1536m2/g；Widen the range of application of activated carbon.
Description
Technical field
The invention belongs to activated carbon preparing technical field, be specifically related to the preparation side of a kind of sucrose base grading-hole activated carbon
Method.
Background technology
Activated carbon is to have the carbonaceous adsorbing material that pore structure is flourishing, specific surface area is big, selective adsorption capacity is strong.?
Under conditions of Yi Ding, a certain or Cucumber of liquid or gas is carried out adsorbing and removing, purifies, refines or reclaim, thus real
Refined and the purification of environment of existing product.Even to this day, activated carbon be widely used in industry, agricultural, national defence, traffic,
The every field such as food, medicine, environmental conservation.The raw material preparing activated carbon at present mainly has Linesless charcoal, wood flour, various shell, coal
Charcoal and the contour carbonaceous material of petroleum coke.The method preparing activated carbon at present conventional has physical activation method, chemical activation method or physics
The method that activation is combined with chemical activation.In physical activation method conventional activated gas be steam, carbon dioxide and they
Mixed gas, will the technique that carries out being reacted to form hole with activated gas of the material with carbon element after carbonization.Chemical activation method be by
After various carbon raw materials uniformly mix with chemical drugs or impregnate, at a suitable temperature, through carbonization, activate and reclaim chemistry
The processes such as medicine produce a kind of method of activated carbon.Chemical activating agent used is usually zinc chloride, phosphoric acid or alkali.Physically activated
After referring to first carbon raw material is carried out carbonization, chemical activation with chemical activation combined techniques, then carry out the further reaming of gas activation.
It is generally acknowledged that the hole of activated carbon is made up of macropore, mesopore and micropore, macropore diameter is 50～2000nm, and mesopore is 2～50nm, micro-
Aperture, hole is less than 2nm.
Although the activated carbon that the method for preparation obtains at present has bigger specific surface area, but mesoporous rate is relatively low, microporosity
Too high, it is unfavorable for the carrying out of some catalytic reactions.Prior art has used multiple method to carry out reaming, such as Chinese patent
(CN1260005C) activated carbon after being disclosed that heat treatment is in the mixing of steam, oxygen-containing gas, nitrogen or noble gas
Atmosphere carries out the heat treatment expanding method of 2-36 hour.But the activated carbon that those expanding methods obtain, however it remains more
Micropore, mesoporous rate is low, and the expanding treatment time is longer, and preparation efficiency is low.
Summary of the invention
It is an object of the invention to provide a kind of sucrose base grading-hole activated carbon to overcome the deficiencies in the prior art
Preparation method.The present invention is with sucrose as raw material, and after sucrose and nickel nitrate being dissolved in water by certain mass ratio, and heating is stirred
Mixing mix homogeneously, more mixed material is carried out carbonization process, after the material after carbonization is removed nickel with hydrochloric acid, washing is dry
Dry, further for material chemical activation is processed, obtain grading-hole activated carbon.The activated carbon that the present invention prepares has classification
Pore structure, its intermediary hole rate reaches 37-52%, microporosity 40-57%, and big porosity is 6-9%；The present invention prepares simultaneously
Activated carbon has high-specific surface area, and specific surface area is up to 1214-1536m2/g；Widen the range of application of activated carbon.
For realizing above-mentioned technical purpose, the technical solution used in the present invention is:
The preparation method of a kind of sucrose base grading-hole activated carbon, comprises the following steps:
Step (1): take sucrose and nickel nitrate is soluble in water, wherein sucrose is 40-50:1 with the mass ratio of nickel nitrate；And in
Stir 30-60min at 80-90 DEG C, after stirring, obtain sucrose nickel nitrate compound；
Step (2): sucrose nickel nitrate compound step (1) obtained is placed in high temperature furnace, under inert atmosphere protection
Carrying out high temperature carbonization, wherein carbonization temperature is 600-800 DEG C, and carbonization time is 1-3h；Obtain material one；
Step (3): adding concentration in the material one step (2) obtained is the hydrochloric acid of 3-6M, the most first stirs 20-
40min, return stirring 15-30min at 50-65 DEG C；It is washed with water after pickling to neutrality, is dried；Obtain material two；
Step (4): adding KOH solution in the material two that step (3) obtains and uniformly mix, wherein material two is with KOH's
Mass ratio is 1:1-4；Place into after baking oven is dried 30-60min at 80-100 DEG C, dried material is put into high temperature furnace
In, high-temperature activation under the protection of inert atmosphere, wherein the temperature of high-temperature activation is 800-1000 DEG C, and the time of high-temperature activation is
1-3h；Obtain material three；
Step (5): the material three step (4) obtained carries out pickling again, is washed to neutrality, obtains grading-hole after drying and lives
Property charcoal.
The further preferred scheme of the preparation method of a kind of sucrose base grading-hole activated carbon that the present invention provides is:
Wherein, in step (1), sucrose is preferably 43-47:1 with the mass ratio of nickel nitrate, more elects 45-47:1 as；Wherein
Sucrose and nickel nitrate are soluble in water, and the temperature of stirring is preferably 85-90 DEG C, and mixing time is preferably 40-50min.
Wherein, the carbonization temperature in step (2) is preferably 700-800 DEG C, and carbonization time is preferably 2-3h；Wherein indifferent gas
Atmosphere is nitrogen, argon or the mixed atmosphere of nitrogen argon.
Wherein, step (3) is preferably 4-6M with concentration of hydrochloric acid, and the temperature of return stirring is preferably 55-60 DEG C, return stirring
Time be preferably 20-30min.
Wherein, step (4) material two is preferably 1:2-4 with the mass ratio of KOH；The temperature of high-temperature activation is preferably 850-
950 DEG C, the time of high-temperature activation is preferably 2-3h.
Wherein, the pickling in step (5) is: adds the hydrochloric acid solution of 1-3M in material three, stirs 30-at normal temperatures
50min；Wherein baking temperature is 100-120 DEG C, and drying time is 5-10h.
The preparation method of a kind of sucrose base grading-hole activated carbon that the present invention proposes, compared with prior art, beneficial effect
For: the activated carbon that the present invention prepares has hierarchical porous structure, and has higher mesoporous rate, and its intermediary hole rate reaches 37-
52%, microporosity is 40-57%.Big porosity is 6-9%；The activated carbon that the present invention prepares simultaneously possesses bigger specific surface
Long-pending, specific surface area reaches 1214-1536m2/g；Widen the range of application of activated carbon.
Detailed description of the invention
Embodiment 1
Step (1): take sucrose and nickel nitrate is soluble in water, wherein sucrose is 40:1 with the mass ratio of nickel nitrate；And in 80
Stir 30min at DEG C, after stirring, obtain sucrose nickel nitrate compound；
Step (2): sucrose nickel nitrate compound step (1) obtained is placed in high temperature furnace, under inert atmosphere protection
Carrying out high temperature carbonization, wherein carbonization temperature is 600 DEG C, and carbonization time is 1h；Obtain material one；
Step (3): adding concentration in the material one step (2) obtained is the hydrochloric acid of 3M, the most first stirs
40min, return stirring 15min at 50 DEG C；It is washed with water after pickling to neutrality, is dried；Obtain material two；
Step (4): adding KOH solution in the material two that step (3) obtains and uniformly mix, wherein material two is with KOH's
Mass ratio is 1:1；Place into after baking oven is dried 30min at 80 DEG C, dried material is put in high temperature furnace, in inertia
High-temperature activation under the protection of atmosphere, wherein the temperature of high-temperature activation is 800 DEG C, and the time of high-temperature activation is 1h；Obtain material three；
Step (5): add the hydrochloric acid solution of 1M in the material three that step (4) obtains, stir 30min at normal temperatures；Again
Wash with water to neutrality, and obtain grading-hole activated carbon after dry 10h at 100 DEG C.
Embodiment 2
Step (1): take sucrose and nickel nitrate is soluble in water, wherein sucrose is 43:1 with the mass ratio of nickel nitrate；And in 85
Stir 40min at DEG C, after stirring, obtain sucrose nickel nitrate compound；
Step (2): sucrose nickel nitrate compound step (1) obtained is placed in high temperature furnace, under inert atmosphere protection
Carrying out high temperature carbonization, wherein carbonization temperature is 700 DEG C, and carbonization time is 2h；Obtain material one；
Step (3): adding concentration in the material one step (2) obtained is the hydrochloric acid of 4M, the most first stirs
30min, return stirring 20min at 55 DEG C；It is washed with water after pickling to neutrality, is dried；Obtain material two；
Step (4): adding KOH solution in the material two that step (3) obtains and uniformly mix, wherein material two is with KOH's
Mass ratio is 1:2；Place into after baking oven is dried 30min at 100 DEG C, dried material is put in high temperature furnace, lazy
High-temperature activation under the protection of property atmosphere, wherein the temperature of high-temperature activation is 850 DEG C, and the time of high-temperature activation is 2h；Obtain material
Three；
Step (5): add the hydrochloric acid solution of 1M in the material three that step (4) obtains, stir 40min at normal temperatures；Again
Wash with water to neutrality, and obtain grading-hole activated carbon after dry 5h at 120 DEG C.
Embodiment 3
Step (1): take sucrose and nickel nitrate is soluble in water, wherein sucrose is 45:1 with the mass ratio of nickel nitrate；And in 85
Stir 50min at DEG C, after stirring, obtain sucrose nickel nitrate compound；
Step (2): sucrose nickel nitrate compound step (1) obtained is placed in high temperature furnace, under inert atmosphere protection
Carrying out high temperature carbonization, wherein carbonization temperature is 750 DEG C, and carbonization time is 2h；Obtain material one；
Step (3): adding concentration in the material one step (2) obtained is the hydrochloric acid of 4M, the most first stirs
30min, return stirring 20min at 60 DEG C；It is washed with water after pickling to neutrality, is dried；Obtain material two；
Step (4): adding KOH solution in the material two that step (3) obtains and uniformly mix, wherein material two is with KOH's
Mass ratio is 1:3；Place into after baking oven is dried 30min at 100 DEG C, dried material is put in high temperature furnace, lazy
High-temperature activation under the protection of property atmosphere, wherein the temperature of high-temperature activation is 950 DEG C, and the time of high-temperature activation is 2h；Obtain material
Three；
Step (5): add the hydrochloric acid solution of 1M in the material three that step (4) obtains, stir 40min at normal temperatures；Again
Wash with water to neutrality, and obtain grading-hole activated carbon after dry 5h at 120 DEG C.
Embodiment 4
Step (1): take sucrose and nickel nitrate is soluble in water, wherein sucrose is 50:1 with the mass ratio of nickel nitrate；And in 90
Stir 60min at DEG C, after stirring, obtain sucrose nickel nitrate compound；
Step (2): sucrose nickel nitrate compound step (1) obtained is placed in high temperature furnace, under inert atmosphere protection
Carrying out high temperature carbonization, wherein carbonization temperature is 800 DEG C, and carbonization time is 3h；Obtain material one；
Step (3): adding concentration in the material one step (2) obtained is the hydrochloric acid of 6M, the most first stirs
20min, return stirring 30min at 65 DEG C；It is washed with water after pickling to neutrality, is dried；Obtain material two；
Step (4): adding KOH solution in the material two that step (3) obtains and uniformly mix, wherein material two is with KOH's
Mass ratio is 1:4；Place into after baking oven is dried 30min at 100 DEG C, dried material is put in high temperature furnace, lazy
High-temperature activation under the protection of property atmosphere, wherein the temperature of high-temperature activation is 1000 DEG C, and the time of high-temperature activation is 3h；Obtain material
Three；
Step (5): add the hydrochloric acid solution of 3M in the material three that step (4) obtains, stir 50min at normal temperatures；Again
Wash with water to neutrality, and obtain grading-hole activated carbon after dry 5h at 120 DEG C.
Performance detects:
The performance measurement result of the activated carbon now embodiment 1-embodiment 4 obtained presents in Table 1, as seen from Table 1
It is mesoporous that the activated carbon that the present invention prepares has grading-hole, and has higher mesoporous rate, and its intermediary hole rate reaches 37-
52%, microporosity 40-57%, big porosity is 6-9%；The activated carbon that the present invention prepares simultaneously has high-specific surface area, than
Surface area is up to 1214-1536m2/g。
The character of the activated carbon that table 1 present invention prepares
The explanation being not directed in the detailed description of the invention of the present invention belongs to techniques well known, refers to known technology and adds
To implement.
The present invention, through validation trial, achieves satisfied trial effect.
Embodiments of the present invention are not limited to above-described embodiment, and that makes on the premise of without departing from present inventive concept is various
Within change belongs to protection scope of the present invention.
Claims (7)
1. the preparation method of a sucrose base grading-hole activated carbon, it is characterised in that comprise the following steps:
Step (1): take sucrose and nickel nitrate is soluble in water, wherein sucrose is 40-50:1 with the mass ratio of nickel nitrate；And in 80-
Stir 30-60min at 90 DEG C, after stirring, obtain sucrose nickel nitrate compound；
Step (2): sucrose nickel nitrate compound step (1) obtained is placed in high temperature furnace, carries out under inert atmosphere protection
High temperature carbonization, wherein carbonization temperature is 600-800 DEG C, and carbonization time is 1-3h；Obtain material one；
Step (3): adding concentration in the material one step (2) obtained is the hydrochloric acid of 3-6M, the most first stirs 20-
40min, return stirring 15-30min at 50-65 DEG C；It is washed with water after pickling to neutrality, is dried；Obtain material two；
Step (4): add KOH solution in the material two that step (3) obtains and uniformly mix, wherein the quality of material two and KOH
Ratio is 1:1-4；Place into after baking oven is dried 30-60min at 80-100 DEG C, dried material put in high temperature furnace,
High-temperature activation under the protection of inert atmosphere, wherein the temperature of high-temperature activation is 800-1000 DEG C, and the time of high-temperature activation is 1-
3h；Obtain material three；
Step (5): the material three step (4) obtained carries out pickling again, is washed to neutrality, obtains grading-hole activity after drying
Charcoal.
The preparation method of a kind of sucrose base grading-hole activated carbon the most according to claim 1, it is characterised in that step (1)
Middle sucrose is preferably 43-47:1 with the mass ratio of nickel nitrate.
The preparation method of a kind of sucrose base grading-hole activated carbon the most according to claim 1, it is characterised in that step (1)
Described in sucrose and nickel nitrate soluble in water, the temperature of stirring is 85-90 DEG C, and mixing time is 40-50min.
The preparation method of a kind of sucrose base grading-hole activated carbon the most according to claim 1, it is characterised in that step (2)
In carbonization temperature be 700-800 DEG C, carbonization time is 2-3h.
The preparation method of a kind of sucrose base grading-hole activated carbon the most according to claim 1, it is characterised in that step (3)
Being 4-6M with concentration of hydrochloric acid, the temperature of return stirring is 55-60 DEG C, and the time of return stirring is 20-30min.
The preparation method of a kind of sucrose base grading-hole activated carbon the most according to claim 1, it is characterised in that step (4)
Middle material two is 1:2-4 with the mass ratio of KOH；The temperature of high-temperature activation is 850-950 DEG C, and the time of high-temperature activation is 2-3h.
The preparation method of a kind of sucrose base grading-hole activated carbon the most according to claim 1, it is characterised in that step (5)
Middle pickling is: adds the hydrochloric acid solution of 1-3M in material three, stirs 30-50min at normal temperatures.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107570157A (en) * | 2017-09-15 | 2018-01-12 | 青岛科技大学 | A kind of preparation method for the order mesoporous Pd/carbon catalyst for preparing p-aminophenol |
| CN110921649A (en) * | 2019-10-31 | 2020-03-27 | 山东理工大学 | Two-dimensional carbon nanosheet and method for preparing two-dimensional carbon nanosheets in large scale |
| CN113652207A (en) * | 2021-08-25 | 2021-11-16 | 云南师范大学 | Adsorptive phase-change material for cold-chain logistics and preparation method thereof |
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| CN102658084A (en) * | 2012-05-18 | 2012-09-12 | 东南大学 | Preparation method of nickel nitrate modified sludge activated carbon |
| CN104916452A (en) * | 2015-04-21 | 2015-09-16 | 中国林业科学研究院林产化学工业研究所 | Wooden active carbon composite material for super capacitor and preparing method of wooden activated carbon composite material |
| CN105217627A (en) * | 2015-10-13 | 2016-01-06 | 福州大学 | A kind of preparation method of coconut husk greying gac |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101585527A (en) * | 2008-05-23 | 2009-11-25 | 中国人民解放军63971部队 | In a kind of being rich in, the charcoal preparation methods of macropore |
| CN102658084A (en) * | 2012-05-18 | 2012-09-12 | 东南大学 | Preparation method of nickel nitrate modified sludge activated carbon |
| CN104916452A (en) * | 2015-04-21 | 2015-09-16 | 中国林业科学研究院林产化学工业研究所 | Wooden active carbon composite material for super capacitor and preparing method of wooden activated carbon composite material |
| CN105217627A (en) * | 2015-10-13 | 2016-01-06 | 福州大学 | A kind of preparation method of coconut husk greying gac |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107570157A (en) * | 2017-09-15 | 2018-01-12 | 青岛科技大学 | A kind of preparation method for the order mesoporous Pd/carbon catalyst for preparing p-aminophenol |
| CN110921649A (en) * | 2019-10-31 | 2020-03-27 | 山东理工大学 | Two-dimensional carbon nanosheet and method for preparing two-dimensional carbon nanosheets in large scale |
| CN110921649B (en) * | 2019-10-31 | 2021-10-22 | 山东理工大学 | Two-dimensional carbon nanosheet and method for preparing two-dimensional carbon nanosheets in large scale |
| CN113652207A (en) * | 2021-08-25 | 2021-11-16 | 云南师范大学 | Adsorptive phase-change material for cold-chain logistics and preparation method thereof |
| CN113652207B (en) * | 2021-08-25 | 2023-11-17 | 云南师范大学 | Adsorptive phase change material for cold chain logistics and preparation method thereof |
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