CN106495152A - The preparation method of activated carbon with high specific surface area - Google Patents
The preparation method of activated carbon with high specific surface area Download PDFInfo
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- CN106495152A CN106495152A CN201611043237.3A CN201611043237A CN106495152A CN 106495152 A CN106495152 A CN 106495152A CN 201611043237 A CN201611043237 A CN 201611043237A CN 106495152 A CN106495152 A CN 106495152A
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- activated carbon
- soapberry
- residue
- surface area
- specific surface
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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
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- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
The present invention relates to technical field of function materials, and in particular to a kind of preparation method of activated carbon with high specific surface area.Extracted the soapberry residue after biodiesel raw material oil to wash, dry, crush through 80% ethanol water, soapberry residue is impregnated using alcohol, the unstable carbonaceous organic material in soapberry residue is removed, the skeleton of activated carbon is enhanced, is obtained charcoal rate and intensity；Then the soapberry residue that handles well is put in microwave reactor, soapberry residue is carbonized；By activated carbon carbonized material and KOH and K2CO3The composite activating agent mixing of composition, takes 10g after grinding is uniform and is put in tube furnace, in N2Carbonized material is activated under protection；After cooling, activated carbon is first soaked 2h with 1 mol/L hydrochloric acid solutions, reusable heat distillation water washing is constant to pH values, is put in 110 DEG C of constant temperature blast drying ovens and dries, obtains final product activated carbon sample.The activated carbon has the specific surface area of superelevation and higher mesopore proportion, can be used for the electrode material of ultracapacitor.
Description
Technical field
The present invention relates to technical field of function materials, and in particular to a kind of preparation method of activated carbon with high specific surface area.
Background technology
Activated carbon as porous adsorbing material, with abundant pore structure, higher specific surface area, excellent absorption
Performance and stable chemical property, are widely used in the fields such as chemical industry, medical treatment, military affairs, environmental protection.However as medicine, environmental protection,
The continuous development in the fields such as military affairs, normal activated carbon (800 ~ 1500 m of specific surface area2/ g) as Selective adsorption is poor, ratio
Surface area is low, adsorption capacity is limited, can not meet the particular/special requirement in these fields, and this is caused to active carbon with high specific surface area
Demand constantly rises.
(abbreviation HSMC, specific surface area are generally higher than 2500 m to activated carbon with high specific surface area2/ g) have specific surface area high,
The advantages of microvoid content is high, pore-size distribution is narrow, adsorbance is big, can be used for double layer capacitor, natural gas storage, reclaim enrichment expensive
The fields such as metal, methane adsorbent, effective catalyst and catalyst carrier.
The raw material for preparing activated carbon has petroleum coke, coal and biomass etc., with the increasingly depleted of non-renewable energy resources,
The agriculture and forestry organic waste materials such as shell, bamboo and wood are due to being just taken as the raw material for preparing activated carbon more and more have the advantages that easily-activated.
Soapberry is particularly Fujian Province in the whole nation and plants energetically as important energy seeds, and soapberry extracts biodiesel raw material
Substantial amounts of residue is left after oil, and containing substantial amounts of cellulose, in residue, the content of carbon is up to 49.34% after testing, abandons
Both welding, and waste of resource.Therefore, preparing activated carbon using soapberry residue can reduce environmental pollution, improve without trouble
The comprehensive utilization value of son.
Content of the invention
The present invention proposes the preparation method that a kind of utilization soapberry residue prepares activated carbon with high specific surface area.
Technical program of the present invention lies in：
The preparation method of activated carbon with high specific surface area, comprises the steps：
Extracted the soapberry residue after biodiesel raw material oil to wash, dry, crush through 80% ethanol water, using alcohol
Dipping soapberry residue, removes the unstable carbonaceous organic material in soapberry residue, enhances the skeleton of activated carbon, obtains charcoal rate
And intensity；
Then the soapberry residue that handles well is put in microwave reactor, soapberry residue is carbonized；
By activated carbon carbonized material and KOH and K2CO3The composite activating agent mixing of composition, takes 10g after grinding is uniform and is put into tubular type
In stove, in N2Carbonized material is activated under protection；
After cooling, activated carbon is first soaked 2h with 1 mol/L hydrochloric acid solutions, reusable heat distillation water washing is constant to pH values, is put into
Dry in 110 DEG C of constant temperature blast drying ovens, obtain final product activated carbon sample.
During described charing, N2Flow is 200 mL/min;Carburizing temperature is 400 DEG C, and microwave power is 800W, during carbonization
Between be 60 min, heating rate be 10 DEG C/min.
Described charing needs N2Protection.
During activation, N2Flow is 200mL/min, insulation, and heating rate is 10 DEG C/min.
Described KOH and K2CO3Mass ratio be 4：1.
The method have technical effect that：
The present invention with soapberry residue as raw material, KOH and K2CO3For composite activating agent, using microwave carbonization and two steps are activated
Method can prepare activated carbon with high specific surface area.It is 4 in alkali carbon ratio：1, activation temperature is 800 DEG C, and soak time is 30min, prepares
Activated carbon methylene blue adsorption value reach 595mg/g;Under the technique, the BET specific surface areas of activated carbon are up to 3597.4 m2/ g,
The accumulative total pore volume of absorption is 1.8204cm3/ g, average pore size are 2.0241nm.The activated carbon have the specific surface area of superelevation and
Higher mesopore proportion, can be used for the electrode material of ultracapacitor.
Specific embodiment
The preparation method of activated carbon with high specific surface area, comprises the steps：
Embodiment 1
Extracted the soapberry residue after biodiesel raw material oil to wash, dry, crush through 80% ethanol water, using alcohol
Dipping soapberry residue, removes the unstable carbonaceous organic material in soapberry residue, enhances the skeleton of activated carbon, obtains charcoal rate
And intensity；Then the soapberry residue that handles well is put in microwave reactor, soapberry residue is carbonized；By activity
Charcoal carbonized material and KOH and K2CO3The composite activating agent mixing of composition, takes 10g after grinding is uniform and is put in tube furnace, in N2Protect
Carbonized material is activated under shield；After cooling, activated carbon is first soaked 2h, reusable heat distillation washing with 1 mol/L hydrochloric acid solutions
Wash constant to pH values, be put in 110 DEG C of constant temperature blast drying ovens dry, obtain final product activated carbon sample.During described charing, N2Stream
Measure as 200 mL/min;Carburizing temperature is 400 DEG C, and microwave power is 800W, and carbonization time is 60 min, and heating rate is 10
℃/min.Described charing needs N2Protection.During activation, N2Flow is 200mL/min, insulation, and heating rate is 10 DEG C/min.
Described KOH and K2CO3Mass ratio be 4：1.
Embodiment 2
Extracted the soapberry residue after biodiesel raw material oil to wash, dry, crush through 85% ethanol water, using alcohol
Dipping soapberry residue, removes the unstable carbonaceous organic material in soapberry residue, enhances the skeleton of activated carbon, obtains charcoal rate
And intensity；Then the soapberry residue that handles well is put in microwave reactor, soapberry residue is carbonized；By activity
Charcoal carbonized material and KOH and K2CO3The composite activating agent mixing of composition, takes 12g after grinding is uniform and is put in tube furnace, in N2Protect
Carbonized material is activated under shield；After cooling, activated carbon is first soaked 3h, reusable heat distillation washing with 1.5mol/L hydrochloric acid solutions
Wash constant to pH values, be put in 120 DEG C of constant temperature blast drying ovens dry, obtain final product activated carbon sample.During described charing, N2Stream
Measure as 180 mL/min;Carburizing temperature is 450 DEG C, and microwave power is 800W, and carbonization time is 60 min, and heating rate is 12
℃/min.Described charing needs N2Protection.During activation, N2Flow is 200mL/min, insulation, and heating rate is 10 DEG C/min.
Described KOH and K2CO3Mass ratio be 4：1.
Claims (5)
1. the preparation method of activated carbon with high specific surface area, it is characterised in that：Comprise the steps：
Extracted the soapberry residue after biodiesel raw material oil to wash, dry, crush through 80% ethanol water, using alcohol
Dipping soapberry residue, removes the unstable carbonaceous organic material in soapberry residue, enhances the skeleton of activated carbon, obtains charcoal rate
And intensity；
Then the soapberry residue that handles well is put in microwave reactor, soapberry residue is carbonized；
By activated carbon carbonized material and KOH and K2CO3The composite activating agent mixing of composition, takes 10g after grinding is uniform and is put into tube furnace
In, in N2Carbonized material is activated under protection；
After cooling, activated carbon is first soaked 2h with 1 mol/L hydrochloric acid solutions, reusable heat distillation water washing is constant to pH values, is put into
Dry in 110 DEG C of constant temperature blast drying ovens, obtain final product activated carbon sample.
2. the preparation method of activated carbon with high specific surface area according to claim 1, it is characterised in that：Described charing
When, N2Flow is 200 mL/min;Carburizing temperature is 400 DEG C, and microwave power is 800W, and carbonization time is 60 min, and heat up speed
Rate is 10 DEG C/min.
3. the preparation method of activated carbon with high specific surface area according to claim 2, it is characterised in that：Described charing is needed
Want N2Protection.
4. the preparation method of activated carbon with high specific surface area according to claim 1, it is characterised in that：Described activation
When, N2Flow is 200mL/min, insulation, and heating rate is 10 DEG C/min.
5. the preparation method of activated carbon with high specific surface area according to claim 1, it is characterised in that：Described KOH and
K2CO3Mass ratio be 4：1.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611043237.3A CN106495152A (en) | 2016-11-24 | 2016-11-24 | The preparation method of activated carbon with high specific surface area |
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| CN201611043237.3A CN106495152A (en) | 2016-11-24 | 2016-11-24 | The preparation method of activated carbon with high specific surface area |
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| CN106495152A true CN106495152A (en) | 2017-03-15 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108910881A (en) * | 2018-08-27 | 2018-11-30 | 天津市职业大学 | A kind of composite activating agent preparing high performance active carbon and its application |
| CN109704333A (en) * | 2019-01-24 | 2019-05-03 | 江苏理工学院 | Durian shell active carbon and preparation method thereof |
| CN109704335A (en) * | 2018-12-24 | 2019-05-03 | 宁波环洋新材料股份有限公司 | A kind of processing method of the bottoms generated in refining crude glycerin |
| CN112421061A (en) * | 2020-10-29 | 2021-02-26 | 电子科技大学 | Method for preparing Fe-N-C oxygen reduction catalyst by taking pig blood as raw material |
| CN113380556A (en) * | 2021-06-08 | 2021-09-10 | 福建师范大学泉港石化研究院 | Nano flaky conductive agent |
-
2016
- 2016-11-24 CN CN201611043237.3A patent/CN106495152A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108910881A (en) * | 2018-08-27 | 2018-11-30 | 天津市职业大学 | A kind of composite activating agent preparing high performance active carbon and its application |
| CN109704335A (en) * | 2018-12-24 | 2019-05-03 | 宁波环洋新材料股份有限公司 | A kind of processing method of the bottoms generated in refining crude glycerin |
| CN109704333A (en) * | 2019-01-24 | 2019-05-03 | 江苏理工学院 | Durian shell active carbon and preparation method thereof |
| CN112421061A (en) * | 2020-10-29 | 2021-02-26 | 电子科技大学 | Method for preparing Fe-N-C oxygen reduction catalyst by taking pig blood as raw material |
| CN113380556A (en) * | 2021-06-08 | 2021-09-10 | 福建师范大学泉港石化研究院 | Nano flaky conductive agent |
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