CN105905895A - Preparation device of nitrogen-containing activated carbon and preparation method - Google Patents
Preparation device of nitrogen-containing activated carbon and preparation method Download PDFInfo
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- CN105905895A CN105905895A CN201610236706.7A CN201610236706A CN105905895A CN 105905895 A CN105905895 A CN 105905895A CN 201610236706 A CN201610236706 A CN 201610236706A CN 105905895 A CN105905895 A CN 105905895A
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Abstract
The invention belongs to the technical field of activated carbon material. A preparation technology of nitrogen-containing activated carbon comprises the following steps: carbonizing a precursor at protective gas atmosphere inside a high temperature pipe furnace; measuring temperature by a temperature measurement probe and controlling temperature of ammonia water inside a closed thermal water kettle to room temperature-99 DEG C; activating the carbonized precursor; letting protective gas pass through the closed thermal water kettle during the activation process, heating through the ammonia water inside the closed thermal water kettle, and letting the space above the liquid level of the ammonia water in the closed thermal water kettle be filled with the protective gas containing ammonia gas and water vapor; letting the protective gas containing ammonia gas and water vapor enter the high temperature pipe furnace; activating the carbonized raw material and the ammonia gas and water vapor at the atmosphere of protective gas; stopping introducing ammonia gas and water vapor after the activation and turning off the high temperature reaction furnace, and cooling to obtain activated carbon fiber rich in nitrogen. The technology is simple to operate and easy to control. Energy consumption is low. In addition, the product has consistent quality and is convenient for promotion and application.
Description
Technical field
The invention belongs to absorbent charcoal material technical field, be specifically related to preparation facilities and the preparation of a kind of nitrogenous activated carbon
Method.
Background technology
Activated carbon rich in nitrogen is that in carbon structure, a part of carbon atom is replaced by nitrogen-atoms, thus has the table of uniqueness
Face chemical property, the most unazotized activated carbon of activated carbon rich in nitrogen has more preferable hydrophily and adsorption capacity,
There are higher absorption property in sulphur system and compound nitrogen series, simultaneously because nitrogen-atoms electronic shell delocalization ability higher because of
And there is higher chemical property.The common preparation method preparing nitrogenous activated carbon at present has template, carbonization/work
Change the method etc. of nitrogenous precursor.The most topmost research is to study different process using nitrogenous precursor as raw material
Impact.
The patent of the preparation method of the entitled nitrogenous activated-carbon catalyst of patent CN102553641B, uses carbonized stock
Strong oxidizer dipping or reflow treatment, be blended with certain proportion with nitrogenous reagent afterwards, moves into high temperature process furnances lazy
Property atmosphere under activate, prepare rich in the activated carbon product of nitrogen.Patent CN102360959A utilizes rich in nitrogen unit
Raw material made by the Lauxite of element, carbonizes, activates system after raw material under an inert atmosphere carbonization after being blended with potassium hydroxide
The activated carbon of standby rich Nitrogen element.It is molten that patent CN103408007A utilizes normal activated carbon or material with carbon element to add ethanol
In liquid, add melamine waste blending and stirring ultrasonically treated, carbonization under inert atmosphere in high temperature furnace afterwards
Activation process, prepares nitrogenous activated carbon.Said method technique is cumbersome, and raw material expensive raw material price, and this work
Skill process is the most simple to operate, and raw material ammonia can recycle, energy-conserving and environment-protective.
Summary of the invention
The problem that present invention aim at existing for prior art, it is provided that the system of the activated carbon of a kind of rich Nitrogen element
Make preparation facilities and preparation method.
Technical scheme is as follows:
The preparation facilities of the nitrogenous activated carbon that the present invention provides, wherein, described device includes:
One high temperature process furnances 10, its port of export is provided with outlet, and arrival end arranges the first entrance and the second entrance；
One protective gas feedway 20 equipped with protective gas；
One closed hot water still 30 equipped with ammoniacal liquor, described closed hot water still 30 stretches out closed equipped with upper port
First vertical pipe 31 and the second vertical pipe 32 of hot water still 30 upper end cover；Stretch to bottom described first vertical pipe 31
In ammoniacal liquor in closed hot water still；Ammoniacal liquor in described closed hot water still is stretched to bottom described second vertical pipe 32
In the upper space of liquid level；
The outlet of described protective gas feedway 20 is connected with the first arm of a threeway；The second of this threeway
Arm is connected by the first entrance of the first switch valve 2 with described high temperature process furnances 10, the 3rd arm of this threeway
It is connected with described the first vertical pipe 31 upper port being placed in closed hot water still 30；Described high temperature process furnances
Second entrance of 10 is connected by second switch valve 3 pipe 32 vertical with second be placed in closed hot water still 30
Logical.
Protective gas feedway of the present invention, it is possible to use all kinds of gas storage device well known in the art,
Such as air accumulator, gas bomb etc..
According to the preparation facilities of the present invention, the most preferably, described protective gas feedway 20 exports by stream
Gauge 4 is connected with the first arm of a threeway.
It is further preferred that described preparation facilities also includes the outlet being installed on described protective gas feedway 20
And the 3rd switch valve 1 connected on pipeline between described flowmeter 4.
According to the preparation facilities of the present invention, the most preferably, described preparation facilities can also include sequentially being communicated in institute
State tail gas filter 40 and the ammonia recycling device 50 of high-temperature tubular outlet of still, the solid particle that course of reaction produces
After refuse is filtered, the ammonia not consumed is collected Posterior circle and utilizes.Described tail gas filter and Ammonia recovery dress
Put and all can use that this area is existing, solid particle refuse can be realized filter the device absorbed with ammonia.
According to the preparation facilities of the present invention, wherein, described preparation facilities can also include being loaded on described closed hot water
In order to thermometric the temperature probe 33 that controls water temperature in still 30.
The preparation method based on above-mentioned nitrogenous activated carbon preparation facilities that the present invention provides, comprises the following steps:
1) carbonization of Precursors of Fibers:
Within Precursors of Fibers is loaded high temperature process furnances, close second switch valve, open the first switch valve, protection
Property gas supply device in protective gas enter high temperature process furnances, high-temperature tubular in-furnace temperature control at 600 DEG C～
1000 DEG C, Precursors of Fibers carries out carbonization in protective gas atmosphere；
2) control described equipped with ammonia temperature in the closed hot water still of ammoniacal liquor normal temperature～99 DEG C；
3) activation of Precursors of Fibers:
After Precursors of Fibers carbonization in high temperature process furnances completes, close the first switch valve, open second switch valve,
Protective gas in protective gas feedway enters the closed hot water still equipped with ammoniacal liquor, at closed hot water still
Ammoniacal liquor heating in it, is full of in space on hot solution liquid level in closed hot water still and carries ammonia and water vapour
Protective gas；This protective gas carrying ammonia and water vapour enters high-temperature tubular by the second switch valve opened
In stove；In high temperature process furnances, Precursors of Fibers, ammonia and water vapour three after carbonization are at protective gas atmosphere
Carry out the activation process of 30～120 minutes at 700～900 DEG C under enclosing；
4), after activation process completes, stop being passed through ammonia and water vapour and closing high temperature reaction stove, contained after cooling
Nitrogen activated carbon.
Preparation in accordance with the present invention, the most preferably, step 1) described in fiber precursor be pitch-based fiber,
Polyacrylonitrile fibre, vinylon, vinal, viscose rayon, bamboo fibre, cotton fiber,
One or more in sisal fiber, monkey grass or natural straw cellulose fibre.
Preparation in accordance with the present invention, wherein, described protective gas be nitrogen, helium, neon, argon gas,
A kind of in Krypton, xenon and radon gas or by several by arbitrary volume than the gaseous mixtures of mixing.
Preparation in accordance with the present invention, the most preferably, the mass concentration of the ammoniacal liquor in described closed hot water still
It is 5%～28%.
Preparation in accordance with the present invention, the most preferably, described protective gas feedway is scored by flow
It is not connected with second switch valve and the first switch valve, manages between the outlet of described protective gas feedway and flowmeter
Equipped with the 3rd switch valve on road, controlled the quantity delivered of protective gas by the 3rd switch valve.
Preparation in accordance with the present invention, the most preferably, described preparation method can also include by being communicated in
The tail gas filter of described high-temperature tubular outlet of still and ammonia recycling device, the solid particle that course of reaction produces gives up
After thing is filtered, the ammonia not consumed is collected Posterior circle and utilizes.
Present invention have the advantage that
The technological process of the present invention is simple, and activation process can be accurate by ammonia temperature in controlling closed hot water still
The content of regulation ammonia, thus regulate the nitrogen content of final products, such that it is able to produce for different Demand Design
The product of different model；There is bigger application value.
Accompanying drawing explanation
Fig. 1 is the preparation technology schematic flow sheet of the nitrogenous activated carbon of the present invention.
Reference
1, the 3rd switch valve the 2, first switch valve 3, second switch valve
4, flowmeter 10, high temperature process furnances 20, protective gas feedway
30, closed hot water still 31, first vertical pipe the 32, second vertical pipe
33, temperature probe 40, tail gas filter 50, ammonia recycling device
Detailed description of the invention
Below in conjunction with specific embodiment, the invention will be further described.
Fig. 1 is the structural representation of the preparation facilities of the nitrogenous activated carbon of one embodiment of the invention, also contains simultaneously
The schematic flow sheet of the preparation method of nitrogen activated carbon.As shown in Figure 1, the preparation facilities of the nitrogenous activated carbon of the present invention,
Comprising:
One high temperature process furnances 10, its port of export is provided with outlet, and arrival end arranges the first entrance and the second entrance；
One protective gas feedway 20 equipped with protective gas；
One closed hot water still 30 equipped with ammoniacal liquor, described closed hot water still 30 stretches out closed equipped with upper port
First vertical pipe 31 and the second vertical pipe 32 of hot water still 30 upper end cover；Stretch to bottom described first vertical pipe 31
In ammoniacal liquor in closed hot water still；Ammoniacal liquor in described closed hot water still is stretched to bottom described second vertical pipe 32
In the upper space of liquid level；
The outlet of described protective gas feedway 20 is connected with the first arm of a threeway；The second of this threeway
Arm is connected by the first entrance of the first switch valve 2 with described high temperature process furnances 10, the 3rd arm of this threeway
It is connected with described the first vertical pipe 31 upper port being placed in closed hot water still 30；Described high temperature process furnances
Second entrance of 10 is connected by second switch valve 3 pipe 32 vertical with second be placed in closed hot water still 30
Logical.
The most preferably, described protective gas feedway 20 exports by flowmeter 4 and the first of a threeway
Arm is connected.It is further preferred that described preparation facilities also includes being installed on described protective gas feedway
The 3rd switch valve 1 connected on pipeline between outlet and the described flowmeter 4 of 20.Described preparation facilities is all right
Including the tail gas filter 40 and the ammonia recycling device 50 that are sequentially communicated in described high-temperature tubular outlet of still.Described system
Standby device can also include being loaded in described closed hot water still 30 in order to thermometric the temperature probe 33 that controls water temperature.
The preparation method of the nitrogenous activated carbon that the present invention provides, its preparation process includes:
1) the steam activation preparation facilities of an above-mentioned activated carbon fibers with micropores is built；
2) carbonization of fiber precursor:
Fiber precursor is loaded within high temperature process furnances 10, in high temperature process furnances 10 temperature control at 600 DEG C～
1000℃；The fiber precursor being loaded in described high temperature process furnances 10 is carried out carbonization treatment: enter at fiber precursor
During row carbonization treatment, close second switch valve 3, open the first switch valve 2, in protective gas feedway 20
Protective gas enter high temperature process furnances 10, fiber precursor enters in the protective gas atmosphere at 600～1000 DEG C
Row carbonization；Described fiber precursor can be pitch-based fiber, polyacrylonitrile fibre, polyvinyl formal fibre
Dimension, vinal, viscose rayon, bamboo fibre, cotton fiber, sisal fiber, monkey grass or natural straw
Cellulose fibre etc..
2) in utilizing temperature probe thermometric and controlling described closed hot water still 30, water temperature is normal temperature～99 DEG C；
3) activation of fiber precursor:
After treating that the fiber precursor carbonization in high temperature process furnances 10 completes, close the first switch valve 2, open second
Switch valve 3, the protective gas in protective gas feedway 20 enters closed hot water by the first vertical pipe 31
Still 30, in closed hot water still 30 ammoniacal liquor heating, overhead of ammoniacal liquor liquid level in closed hot water still 30 in it
The interior full protective gas carrying ammonia and water vapour；This carries the ammonia protective gas with water vapour by opening
Second switch valve 3 and the second entrance of high temperature process furnances 10 enter in high temperature process furnances 10；At high temperature process furnances
The interior fiber precursor after carbonization is carried out under ammonia and water vapour protective gas atmosphere with carrying at 700～900 DEG C
The activation process of 30～120 minutes:
4), after activation process completes, stop being passed through ammonia and water vapour and closing high temperature reaction stove 10, obtain after cooling
Activated carbon fibers with micropores.
Described protective gas is the one in nitrogen, helium, neon, argon gas, Krypton, xenon and radon gas or several
The gas arbitrary volume planted is than the gaseous mixture of mixing.
Described protective gas feedway 20 exports between described flowmeter 4 on pipeline equipped with the 3rd switch valve 1,
The quantity delivered of protective gas is controlled by the 3rd switch valve 1.
Described preparation process also includes the tail gas filter 40 by being communicated in the outlet of described high temperature process furnances 10
The solid particle refuse producing high temperature process furnances 10 filters, and the ammonia having neither part nor lot in reaction after filtration is by ammonia
Retracting device 50 recycling.
From the foregoing, it will be observed that the ammonia of the activated carbon fibers with micropores of the present invention and steam activation preparation method and preparation facilities,
The core of technical scheme is: prepare the ammonia required for the activation process of NACF with water vapour by protectiveness
Gas is carried along into；Its preparation facilities has only to a protective gas and provides device, and protective gas passes through flow
Being connected with an arm of three-way pipe after meter and communicate, second arm of three-way pipe is passed through the liquid of closed hot water still
Below face, the ammoniacal liquor that the 3rd arm is passed directly in high temperature process furnances, gas and closed hot water still 30 fully connects
After touch access high temperature process furnances 10, carbonisation close second switch valve 3, open the first switch valve 2, make 600～
Carbonisation at 1000 DEG C is carried out in protective gas atmosphere；Activation process closes the first switch valve 2, opens second and opens
Close valve 3, make protective gas carry certain ammonia and enter high temperature process furnances with moisture, after ammonia and steam are to carbonization
Fiber material carries out the activation of 30～120 minutes at 700～900 DEG C.
Activation process, closes the first switch valve 2, opens second switch valve 3, and protective gas is passed through underwater in still
Certain distance, makes gas and water carry certain moisture after being fully contacted and is exported discharge by the upper gas of still and import height
In temperature reacting furnace；Temperature probe can be utilized to control the temperature of water in closed hot water still 30, adjust control as required
Water temperature processed is between normal temperature～99 DEG C, and the ammonia that temperature difference protective gas is carried by is different from moisture,
Temperature is the highest, and the ammonia being passed through in high temperature reaction stove is the highest with vapour content.
Present device device is simple, and technique is easily controlled, and energy consumption is little, and product quality is homogeneous, has bigger pushing away
Wide using value.
Certainly, the present invention can also have various embodiments, in the case of without departing substantially from present invention spirit and essence thereof,
Those of ordinary skill in the art can make various corresponding change and deformation according to disclosure of the invention, but these phases
The change answered and deformation all should belong to the protection domain of appended claims of the invention.
Claims (9)
1. the preparation facilities of a nitrogenous activated carbon, it is characterised in that described device includes:
One high temperature process furnances (10), its port of export is provided with outlet, and arrival end arranges the first entrance and the second entrance；
One protective gas feedway (20) equipped with protective gas；
One closed hot water still (30) equipped with ammoniacal liquor, described closed hot water still (30) is stretched out equipped with upper port
First vertical pipe (31) of closed hot water still (30) upper end cover and the second vertical pipe (32)；Described first vertical
Pipe (31) bottom stretches in the ammoniacal liquor in closed hot water still；Described second vertical pipe (32) bottom stretches to
In described closed hot water still in the upper space of ammoniacal liquor liquid level；
The outlet of described protective gas feedway (20) is connected with the first arm of a threeway；This threeway
Second arm is connected by the first entrance of the first switch valve (2) with described high temperature process furnances (10), this threeway
The 3rd arm be connected with described the first vertical pipe (31) upper port being placed in closed hot water still (30)；
Second entrance of described high temperature process furnances (10) passes through second switch valve (3) and is placed in closed hot water still (30)
The second interior vertical pipe (32) is connected.
Preparation facilities the most according to claim 1, it is characterised in that described protective gas feedway (20
Outlet be connected with the first arm of a threeway by flowmeter (4)；As preferably, described preparation facilities
Also include the connecting tube being installed between the outlet of described protective gas feedway (20) and described flowmeter (4)
The 3rd switch valve (1) on road.
Preparation facilities the most according to claim 1 and 2, it is characterised in that described preparation facilities also includes suitable
The secondary tail gas filter (40) being communicated in described high-temperature tubular outlet of still and ammonia recycling device (50), reacted
After the solid particle refuse that journey produces is filtered, the ammonia not consumed is collected Posterior circle and utilizes.
Preparation facilities the most according to claim 1 and 2, it is characterised in that described preparation facilities also includes dress
Temperature probe (33) in described closed hot water still (30).
5. a preparation method for nitrogenous activated carbon based on preparation facilities described in claim 1, comprises the following steps:
1) carbonization of Precursors of Fibers:
Within Precursors of Fibers is loaded high temperature process furnances, close second switch valve, open the first switch valve, protection
Property gas supply device in protective gas enter high temperature process furnances, high-temperature tubular in-furnace temperature control 600～
1000 DEG C, Precursors of Fibers carries out carbonization in protective gas atmosphere；
2) control described equipped with ammonia temperature in the closed hot water still of ammoniacal liquor normal temperature～99 DEG C；
3) activation of Precursors of Fibers:
After Precursors of Fibers carbonization in high temperature process furnances completes, close the first switch valve, open second switch valve,
Protective gas in protective gas feedway enters the closed hot water still equipped with ammoniacal liquor, at closed hot water still
Ammoniacal liquor heating in it, is full of in space on hot solution liquid level in closed hot water still and carries ammonia and water vapour
Protective gas；This protective gas carrying ammonia and water vapour enters high-temperature tubular by the second switch valve opened
In stove；In high temperature process furnances, Precursors of Fibers, ammonia and water vapour three after carbonization are at protective gas atmosphere
Carry out the activation process of 30～120 minutes at 700～900 DEG C under enclosing；
4), after activation process completes, stop being passed through ammonia and water vapour and closing high temperature reaction stove, contained after cooling
Nitrogen activated carbon.
Preparation method the most according to claim 5, it is characterised in that described fiber precursor is asphaltic base
Fiber, polyacrylonitrile fibre, vinylon, vinal, viscose rayon, bamboo fibre,
One or more in cotton fiber, sisal fiber, monkey grass or natural straw cellulose fibre.
Preparation method the most according to claim 5, it is characterised in that described protective gas is nitrogen, helium
A kind of in gas, neon, argon gas, Krypton, xenon and radon gas or by several by arbitrary volume than the gaseous mixtures of mixing.
Preparation method the most according to claim 5, it is characterised in that the ammoniacal liquor in described closed hot water still
Mass concentration be 5%～28%.
9. according to the arbitrary described preparation method of claim 5-8, it is characterised in that described protective gas supplies
Device is connected with second switch valve and the first switch valve respectively by flowmeter, and described protective gas feedway goes out
Equipped with the 3rd switch valve on pipeline between mouth and flowmeter, controlled the quantity delivered of protective gas by the 3rd switch valve.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108064215A (en) * | 2017-09-08 | 2018-05-22 | 南京林业大学 | A kind of method that ammonia activation prepares nitrogenous activated carbon |
| CN108726503A (en) * | 2018-09-04 | 2018-11-02 | 南京农业大学 | A kind of porous carbon materials Ammonia reforming apparatus |
| CN109264694A (en) * | 2018-10-16 | 2019-01-25 | 蚌埠学院 | The preparation method and device of melamine based porous materials |
| CN109304196A (en) * | 2017-07-27 | 2019-02-05 | 中国石油化工股份有限公司 | One kind carbon material containing hetero atom and its preparation method and application and a kind of hydrocarbon oxidative dehydrogenation processes |
| CN114956079A (en) * | 2022-06-27 | 2022-08-30 | 浙江农林大学 | Method for preparing activated carbon by wood biomass ammonia baking pretreatment |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109304196A (en) * | 2017-07-27 | 2019-02-05 | 中国石油化工股份有限公司 | One kind carbon material containing hetero atom and its preparation method and application and a kind of hydrocarbon oxidative dehydrogenation processes |
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| CN108726503A (en) * | 2018-09-04 | 2018-11-02 | 南京农业大学 | A kind of porous carbon materials Ammonia reforming apparatus |
| CN108726503B (en) * | 2018-09-04 | 2024-05-28 | 南京农业大学 | Porous carbon material high temperature ammonia modifying device |
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| CN114956079A (en) * | 2022-06-27 | 2022-08-30 | 浙江农林大学 | Method for preparing activated carbon by wood biomass ammonia baking pretreatment |
| CN114956079B (en) * | 2022-06-27 | 2024-03-08 | 浙江农林大学 | Method for preparing activated carbon by baking pretreatment of woody biomass ammonia |
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Application publication date: 20160831 |