CN106629721A - Method for safely producing nitrogen-containing super activated carbon - Google Patents
Method for safely producing nitrogen-containing super activated carbon Download PDFInfo
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- CN106629721A CN106629721A CN201611192801.8A CN201611192801A CN106629721A CN 106629721 A CN106629721 A CN 106629721A CN 201611192801 A CN201611192801 A CN 201611192801A CN 106629721 A CN106629721 A CN 106629721A
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- activated carbon
- koh
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- charcoal
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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
Abstract
The invention discloses a method for safely producing nitrogen-containing super activated carbon. The method comprises the step of feeding ammonia gas in a KOH activation process for activation; reaction between the ammonia gas and carbon at high temperature can be used for producing a developed pore structure; furthermore, reaction between the ammonia gas and potassium can be used for solving the problem of difficult release of the potassium in the KOH activation process, and the aim of doping a nitrogen element into the surface of activated carbon is fulfilled. By the adoption of the method, the nitrogen-containing activated carbon with a high specific surface area can be prepared, and the severe production safety problem caused by production and release of elemental potassium in the process of activating KOH to produce the super activated carbon can be solved; a new technical way is supplied to industrial production of the super activated carbon through a KOH activation method.
Description
Technical field
The invention belongs to chemical production technical field, and in particular to a kind of method of the nitrogenous super-activated carbon of safety in production.
Background technology
Activated carbon is that one kind has highly developed pore structure and high-specific surface area (generally in 800～1500m2Between/g)
Excellent carbon absorbent, be widely used to the numerous areas such as environmental protection, chemical industry, food and military project.Super-activated carbon is a class
Specific surface area is more than 2000m2The novel porous matter Carbon Materials of/g, it is carried in super electrode material for electric double layer capacitor, catalyst
Have broad application prospects in the fields such as body, gas separation, hydrogen and natural gas storing material.Therefore, super-activated carbon has been
Become the novel charcoal material competitively developed in Jin20Nian Lai worlds Carbon Materials industry.The master of active carbon with high specific surface area is prepared at present
Method is wanted to be chemistry for activation method, chemical reagent mainly includes alkali metal compound, such as KOH, NaOH and K2CO3, wherein activating
Effect it is best for KOH.Therefore when super-activated carbon is prepared, KOH activation methods are adopted mostly.Although KOH activates carbonaceous forerunner
Body can prepare the longer research history of super-activated carbon, but its Industrialized processing technique does not also make a breakthrough.Wherein hinder
The key issue for hindering KOH activation methods production super-activated carbon is in KOH activation processs, to have substantial amounts of simple substance potassium and generate.And
The activation temperature of KOH activation has exceeded the boiling point of potassium, therefore the industrialized production mistake of super-activated carbon typically at 800 DEG C or so
Cheng Zhong, has substantial amounts of simple substance potassium effusion activation furnace.Potassium is a kind of very active metal simple-substance, runs into moisture in air just
Generation hydrogen can be reacted, and discharges substantial amounts of heat, so that producing blast, to super-activated carbon production huge peace be brought
Full hidden danger.Meanwhile, during effusion, meeting partial condensation blocks pipeline to simple substance potassium in the pipeline of activation furnace, also can be to safety
Production brings hidden danger.Therefore, it is simple substance potassium in safe handling KOH activation processs using the production key technology of super-activated carbon
Release problem.
The main method of ruthenium ammonia synthesis catalyst is to introduce new hetero atom in activated carbon surface and regulate and control it on surface
Existing way.In activated carbon surface nitrogen doped, application performance of the activated carbon in terms of electrochemistry can be significantly improved.Wherein
Most noticeable, the nitrogen that adulterates can significantly improve the performance of the storing up electricity capacity and catalytic oxygen reduction of activated carbon, because
This, the activated carbon of the nitrogen that adulterates has very big application potential in terms of ultracapacitor and fuel cell, the activity of the nitrogen that adulterates
Charcoal, the nitrogen activated carbon that especially adulterates becomes the focus of field of charcoal material research and development, and nitrating activated carbon is also that countries in the world are sent out
The new high-tech product of exhibition.
On the basis of conventional research and development, in order to solve KOH activation processs in the series of security that brought of K released
Production problem, the present inventor applied and obtain 2 patents of invention (ZL200810243618.5,
ZL201010588664.6) authorize.Still need on this basis to more safe ready control KOH activation processs in Potassium release with
And the aspect such as final products performance makes more preferable innovation and creation.
The content of the invention
The technical problem to be solved is the safe practice of nitrogenous super-activated carbon, there is provided one kind safety in production contains
The method of nitrogen super activated carbon, more not only can control Potassium release in KOH activation processs by safe ready, and can prepare
Go out nitrogenous active carbon with high specific surface area product；Technology is simple and cost is cheaper.
To solve above-mentioned technical problem, the technical solution used in the present invention is as follows：
A kind of method of nitrogenous super-activated carbon of keeping the safety in production, comprises the following steps：
(1) carbonaceous raw material and KOH are fitted in reactor, in being then placed in activation furnace tank body, and are passed through noble gases；
(2) after being warming up to 300 DEG C, ammonia is passed through, then heats to activation temperature, activated；
(3) after activation is finished, cooling activation furnace tank body is passed through air to less than 300 DEG C in ammonia, continues to cool down；
(4) after the cooling of activation furnace tank body, activated material is taken out, with Water Sproading KOH and its derivant.
The method of the described nitrogenous super-activated carbon of safety in production, the carbon feedstock for being used is selected from carbonized material, coal, oil
Burnt, coal tar and activated carbon.Carbonized material comes from the carbonized material of Linesless charcoal, coconut husk charcoal, bamboo charcoal and shell class raw material.
The method of the described nitrogenous super-activated carbon of safety in production, KOH is 1-3 with raw material charcoal mass ratio：1.
The method of the described nitrogenous super-activated carbon of safety in production, activation temperature is 800-950 DEG C.
In step (1), noble gases are nitrogen or argon.
In step (2), after being warming up to 300 DEG C with the heating rate of 5K/min, ammonia is passed through, constant temperature 2h is then heated to
Activation temperature, activates 2h.
In step (3), after activation is finished, activation furnace tank body is cooled down under ammonia atmosphere to less than 300 DEG C, led in ammonia
Enter air, continue to be cooled to less than 100 DEG C.
In step (4), activated material is washed with water, and with the fire door and condensing tube in water flushing body of heater, reclaim KOH and its derive
Thing.
Beneficial effect：Compared with prior art, the present invention has following outstanding advantages：
1) in KOH activation processs, the doping vario-property of activation and nitrogen has been synchronously completed, has realized one-step method preparation and contain
Nitrogen active carbon with high specific surface area, reduces the production craft step of nitrogenous activated carbon.
2) using the reaction of ammonia under high temperature and simple substance potassium, the control of simple substance K released can at ambient pressure be realized, it is to avoid
The side effect brought using elevated pressures and the other solid reagents of addition.The peace of KOH activation processs can efficiently be solved
Full production key technical problem.
3) alkali charcoal ratio is significantly reduced, that is, reduces the consumption of KOH.Conventional KOH activation prepares active carbon with high specific surface area
Alkali charcoal ratio will generally reach 4:1, can be in 1-2 using the technology of the present invention：Specific surface area is prepared under 1 alkali charcoal ratio to be more than
2000m2The active carbon with high specific surface area of/g.Substantially reducing for alkali charcoal ratio, can reduce consumption and the subsequent recovery workshop section of KOH
Water consumption and produce load.
4) Safe production method of the invention, with activation efficiency height, equipment relatively simple, the more low remarkable advantage of energy consumption,
It is easy to the industrialized production of KOH activation methods production super-activated carbon and the industrial applications of super-activated carbon.
Specific embodiment
According to following embodiments, the present invention may be better understood.However, as it will be easily appreciated by one skilled in the art that real
Apply the specific material proportion described by example, process conditions and its result and be merely to illustrate the present invention, and also will not should not limit
The present invention described in detail in claims processed.
Embodiment 1
By Linesless charcoal and KOH according to 1:After 1 ratio mixing, in being put into reactor.And nitrogen is passed through, with the intensification of 5K/min
To 300 DEG C, constant temperature is passed through ammonia to ramp after 2 hours, and rises to 850 DEG C with the heating rate of 3K/min, activates 2 hours.
Then less than 300 DEG C are cooled under ammonia atmosphere, air are passed through and ammonia gas mixture body is continued to be cooled to less than 100 DEG C, beaten
Blow-on door, releases reactor, takes out activated material.Wash activated material with water, and the fire door that rinsed in body of heater with water and condensing tube, so as to
Reach the purpose for reclaiming KOH.After reclaiming KOH, then with water rinse-active charcoal more than 5 times, Product Activity charcoal is produced in drying.Activity
The pore structure of charcoal the results are shown in Table 1 with constituent content analysis.Using the processing method of the present invention, do not have in activation heel row feed channel
It was found that simple substance potassium is present, there is not simple substance potassium and be dissolved in water the specific phenomenon of reaction, reach the purpose of safety in production.
Embodiment 2
By Linesless charcoal and KOH according to 2:After 1 ratio mixing, in being put into reactor.And nitrogen is passed through, with the intensification of 5K/min
To 300 DEG C, constant temperature is passed through ammonia to ramp after 2 hours, and rises to 850 DEG C with the heating rate of 3K/min, activates 2 hours.
Then less than 300 DEG C are cooled under ammonia atmosphere, air are passed through and ammonia gas mixture body is continued to be cooled to less than 100 DEG C, beaten
Blow-on door, releases reactor, takes out activated material.Wash activated material with water, and the fire door that rinsed in body of heater with water and condensing tube, so as to
Reach the purpose for reclaiming KOH.After reclaiming KOH, then with water rinse-active charcoal more than 5 times, Product Activity charcoal is produced in drying.Activity
The pore structure of charcoal the results are shown in Table 1 with constituent content analysis.Using the processing method of the present invention, do not have in activation heel row feed channel
It was found that simple substance potassium is present, there is not simple substance potassium and be dissolved in water the specific phenomenon of reaction, reach the purpose of safety in production.
Embodiment 3
By petroleum coke and KOH according to 2:After 1 ratio mixing, in being put into reactor.And nitrogen is passed through, with the liter of 5K/min
To 300 DEG C, constant temperature is passed through ammonia to warm ramp after 2 hours, and rises to 800 DEG C with the heating rate of 3K/min, and activation 2 is little
When.Then less than 300 DEG C are cooled under ammonia atmosphere, air are passed through and ammonia gas mixture body is continued to be cooled to less than 100 DEG C,
Fire door is opened, reactor is released, activated material is taken out.Wash activated material with water, and the fire door that rinsed in body of heater with water and condensing tube, from
And reach the purpose for reclaiming KOH.After reclaiming KOH, then with water rinse-active charcoal more than 5 times, Product Activity charcoal is produced in drying.It is living
Property charcoal pore structure and constituent content analysis the results are shown in Table 1.Using the processing method of the present invention, do not have in activation heel row feed channel
The presence of simple substance potassium is found, simple substance potassium is not occurred and is dissolved in water the specific phenomenon of reaction, reach the purpose of safety in production.
Embodiment 4
By Linesless charcoal and KOH according to 1:After 1 ratio mixing, in being put into reactor.And nitrogen is passed through, with the intensification of 5K/min
To 300 DEG C, constant temperature is passed through ammonia to ramp after 2 hours, and rises to 900 DEG C with the heating rate of 3K/min, activates 2 hours.
Then less than 300 DEG C are cooled under ammonia atmosphere, air are passed through and ammonia gas mixture body is continued to be cooled to less than 100 DEG C, beaten
Blow-on door, releases reactor, takes out activated material.Wash activated material with water, and the fire door that rinsed in body of heater with water and condensing tube, so as to
Reach the purpose for reclaiming KOH.After reclaiming KOH, then with water rinse-active charcoal more than 5 times, Product Activity charcoal is produced in drying.Activity
The pore structure of charcoal the results are shown in Table 1 with constituent content analysis.Using the processing method of the present invention, do not have in activation heel row feed channel
It was found that simple substance potassium is present, there is not simple substance potassium and be dissolved in water the specific phenomenon of reaction, reach the purpose of safety in production.
Embodiment 5
By Linesless charcoal and KOH according to 1:After 1 ratio mixing, in being put into reactor.And nitrogen is passed through, with the intensification of 5K/min
To 300 DEG C, constant temperature is passed through ammonia to ramp after 2 hours, and rises to 950 DEG C with the heating rate of 3K/min, activates 2 hours.
Then less than 300 DEG C are cooled under ammonia atmosphere, air are passed through and ammonia gas mixture body is continued to be cooled to less than 100 DEG C, beaten
Blow-on door, releases reactor, takes out activated material.Wash activated material with water, and the fire door that rinsed in body of heater with water and condensing tube, so as to
Reach the purpose for reclaiming KOH.After reclaiming KOH, then with water rinse-active charcoal more than 5 times, Product Activity charcoal is produced in drying.Activity
The pore structure of charcoal the results are shown in Table 1 with constituent content analysis.Using the processing method of the present invention, do not have in activation heel row feed channel
It was found that simple substance potassium is present, there is not simple substance potassium and be dissolved in water the specific phenomenon of reaction, reach the purpose of safety in production.
Embodiment 6
By coconut husk charcoal and KOH according to 1:After 1 ratio mixing, in being put into reactor.And nitrogen is passed through, with the liter of 5K/min
To 300 DEG C, constant temperature is passed through ammonia to warm ramp after 2 hours, and rises to 900 DEG C with the heating rate of 3K/min, and activation 2 is little
When.Then less than 300 DEG C are cooled under ammonia atmosphere, air is passed through, continue to be cooled to less than 100 DEG C, open fire door, released
Reactor, takes out activated material.Wash activated material with water, and with the fire door and condensing tube in water flushing body of heater, so as to reach KOH is reclaimed
Purpose.After reclaiming KOH, then with water rinse-active charcoal more than 5 times, Product Activity charcoal is produced in drying.The hole knot of activated carbon
Structure the results are shown in Table 1 with constituent content analysis.Using the processing method of the present invention, in activation heel row feed channel simple substance potassium is not found
Exist, simple substance potassium do not occur and be dissolved in water the specific phenomenon of reaction, reach the purpose of safety in production.
Embodiment 7
By Linesless charcoal and KOH according to 2:After 1 ratio mixing, in being put into reactor.And nitrogen is passed through, with the intensification of 5K/min
To 300 DEG C, constant temperature is passed through ammonia to ramp after 2 hours, and rises to 900 DEG C with the heating rate of 3K/min, activates 2 hours.
Then less than 300 DEG C are cooled under ammonia atmosphere, air and ammonia gas mixture body is passed through, continue to be cooled to less than 100 DEG C, beaten
Blow-on door, releases reactor, takes out activated material.Wash activated material with water, and the fire door that rinsed in body of heater with water and condensing tube, so as to
Reach the purpose for reclaiming KOH.After reclaiming KOH, then with water rinse-active charcoal more than 5 times, finally drying obtains activated carbon product.It is living
Property charcoal pore structure and constituent content analysis the results are shown in Table 1.Using the processing method of the present invention, do not have in activation heel row feed channel
The presence of simple substance potassium is found, simple substance potassium is not occurred and is dissolved in water the specific phenomenon of reaction, reach the purpose of safety in production.
Comparative example 1
By Linesless charcoal and KOH according to 2:After 1 ratio mixing, in being put into reactor.And nitrogen is passed through, with the intensification of 5K/min
To 300 DEG C, constant temperature continues to rise to 850 DEG C with the heating rate of 3K/min in a nitrogen atmosphere, activation 2 ramp after 2 hours
Hour.Then less than 100 DEG C are cooled in a nitrogen atmosphere, reactor is released, and take out activated material.Wash activated material with water, be used in combination
Fire door and condensing tube that water is rinsed in body of heater.After reclaiming KOH, then with water rinse-active charcoal more than 5 times, product work is produced in drying
Property charcoal.The pore structure of activated carbon the results are shown in Table 1 with constituent content analysis.After activation, find in activation furnace wall and discharge duct
With the presence of simple substance potassium, occurs the phenomenon of simple substance potassium and water vapor in air reaction when opening fire door.
Comparative example 2
By Linesless charcoal and KOH according to 2:After 1 ratio mixing, in being put into reactor.And nitrogen is passed through, with the intensification of 5K/min
To 300 DEG C, constant temperature continues to rise to 850 DEG C with the heating rate of 3K/min under ammonia ramp after 2 hours, and activation 2 is little
When.Then less than 100 DEG C are cooled in a nitrogen atmosphere, reactor is released, and take out activated material.Wash activated material with water, and use water
The fire door rinsed in body of heater and condensing tube.After reclaiming KOH, then with water rinse-active charcoal more than 5 times, Product Activity is produced in drying
Charcoal.The pore structure of activated carbon the results are shown in Table 1 with constituent content analysis.After activation, find have in activation furnace wall and discharge duct
Simple substance potassium is present, occur the phenomenon of simple substance potassium and water vapor in air reaction when opening fire door.
Comparative example 3
By Linesless charcoal and KOH according to 2:After 1 ratio mixing, in being put into reactor.And nitrogen is passed through, with the intensification of 5K/min
To 300 DEG C, constant temperature continues to rise to 850 DEG C with the heating rate of 3K/min under a nitrogen ramp after 2 hours, and activation 2 is little
When.Then less than 300 DEG C are cooled under ammonia atmosphere, air and ammonia gas mixture body is passed through, continue to be cooled to 100 DEG C with
Under, fire door is opened, reactor is released, take out activated material.Wash activated material with water, and the fire door that rinsed in body of heater with water and condensation
Pipe.After reclaiming KOH, then with water rinse-active charcoal more than 5 times, Product Activity charcoal is produced in drying.The pore structure of activated carbon with
Constituent content analysis the results are shown in Table 1.After activation, do not find that simple substance potassium is present in activation furnace wall and discharge duct.
The yield of the activated carbon of table 1, nitrogen element content and pore structure data
| Yield (%) | Nitrogen element content (%) | Specific surface area (m2/g) | Specific pore volume accumulates (cm3/g) | |
| Embodiment 1 | 65.2 | 3.4 | 2112 | 1.135 |
| Embodiment 2 | 54.8 | 3.7 | 2879 | 1.554 |
| Embodiment 3 | 67.9 | 3.5 | 2318 | 1.115 |
| Embodiment 4 | 56.3 | 4.1 | 2584 | 1.383 |
| Embodiment 5 | 35.1 | 4.2 | 3067 | 1.771 |
| Embodiment 6 | 58.0 | 3.5 | 2483 | 1.298 |
| Embodiment 7 | 32.5 | 3.9 | 3426 | 1.880 |
| Comparative example 1 | 63.9 | 0.31 | 2068 | 1.099 |
| Comparative example 2 | 60.2 | 2.6 | 2647 | 1.441 |
| Comparative example 3 | 63.0 | 1.3 | 2265 | 1.278 |
Claims (9)
1. the method for the nitrogenous super-activated carbon of a kind of safety in production, it is characterised in that comprise the following steps：
（1）Carbonaceous raw material and KOH are fitted in reactor, in being then placed in activation furnace tank body, and noble gases is passed through；
（2）After being warming up to 300 DEG C, ammonia is passed through, then heats to activation temperature, activated；
（3）After activation is finished, cooling activation furnace tank body is passed through air to less than 300 DEG C in ammonia, continues to cool down；
（4）After the cooling of activation furnace tank body, activated material is taken out, with Water Sproading KOH and its derivant.
2. the method for the nitrogenous super-activated carbon of safety in production according to claim 1, it is characterised in that the charcoal for being used is former
Material is selected from carbonized material, coal, petroleum coke, coal tar and activated carbon.
3. the method for the nitrogenous super-activated carbon of safety in production according to claim 1, it is characterised in that KOH and raw material charcoal
Mass ratio is 1-3：1.
4. the method for the nitrogenous super-activated carbon of safety in production according to claim 1, it is characterised in that activation temperature is
800-950℃。
5. the method for the nitrogenous super-activated carbon of safety in production according to claim 2, it is characterised in that carbonized material be from
In the carbonized material of Linesless charcoal, coconut husk charcoal, bamboo charcoal and shell class raw material.
6. the method for the nitrogenous super-activated carbon of safety in production according to claim 1, it is characterised in that step（1）In, it is lazy
Property gas be nitrogen or argon.
7. the method for the nitrogenous super-activated carbon of safety in production according to claim 1, it is characterised in that step（2）In, with
After the heating rate of 5K/min is warming up to 300 DEG C, ammonia is passed through, constant temperature 2h then heats to activation temperature, activates 2h.
8. the method for the nitrogenous super-activated carbon of safety in production according to claim 1, it is characterised in that step（3）In, it is living
After change is finished, activation furnace tank body is cooled down under ammonia atmosphere to less than 300 DEG C, air is passed through in ammonia, continue to be cooled to 100
Below DEG C.
9. the method for the nitrogenous super-activated carbon of safety in production according to claim 1, it is characterised in that step（4）In, use
Washing activated material, and with the fire door and condensing tube in water flushing body of heater, reclaim KOH and its derivant.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108392942A (en) * | 2018-03-16 | 2018-08-14 | 东华大学 | A kind of amino modified alkali metal base CO2Adsorbent and preparation method thereof |
| CN110092377A (en) * | 2018-01-31 | 2019-08-06 | 东华理工大学 | It is a kind of using Cuttlefish Ink as nitrogen-doped nanometer hole carbosphere of raw material and preparation method thereof |
| CN111540617A (en) * | 2020-06-09 | 2020-08-14 | 华中农业大学 | Preparation system and method of straw nitrogen-phosphorus-iron co-doped active carbon electrode material |
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| CN101993071A (en) * | 2010-12-15 | 2011-03-30 | 南京林业大学 | Method and device for producing super active carbon |
| CN104150479A (en) * | 2014-07-17 | 2014-11-19 | 大连理工大学 | Preparation method of doped high-specific-surface-area activated carbon |
| CN104525110A (en) * | 2014-12-18 | 2015-04-22 | 华中科技大学 | Nitrogen-enriched active biomass coke and preparation method thereof |
| CN105280930A (en) * | 2015-05-18 | 2016-01-27 | 深圳市国创新能源研究院 | Activated carbon material for cathode reaction and preparation method |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101993071A (en) * | 2010-12-15 | 2011-03-30 | 南京林业大学 | Method and device for producing super active carbon |
| CN104150479A (en) * | 2014-07-17 | 2014-11-19 | 大连理工大学 | Preparation method of doped high-specific-surface-area activated carbon |
| CN104525110A (en) * | 2014-12-18 | 2015-04-22 | 华中科技大学 | Nitrogen-enriched active biomass coke and preparation method thereof |
| CN105280930A (en) * | 2015-05-18 | 2016-01-27 | 深圳市国创新能源研究院 | Activated carbon material for cathode reaction and preparation method |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110092377A (en) * | 2018-01-31 | 2019-08-06 | 东华理工大学 | It is a kind of using Cuttlefish Ink as nitrogen-doped nanometer hole carbosphere of raw material and preparation method thereof |
| CN108392942A (en) * | 2018-03-16 | 2018-08-14 | 东华大学 | A kind of amino modified alkali metal base CO2Adsorbent and preparation method thereof |
| CN111540617A (en) * | 2020-06-09 | 2020-08-14 | 华中农业大学 | Preparation system and method of straw nitrogen-phosphorus-iron co-doped active carbon electrode material |
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Application publication date: 20170510 |