CN107915226A - A kind of preparation method and device of hydrogen-free absorbent charcoal material - Google Patents
A kind of preparation method and device of hydrogen-free absorbent charcoal material Download PDFInfo
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- CN107915226A CN107915226A CN201711320171.2A CN201711320171A CN107915226A CN 107915226 A CN107915226 A CN 107915226A CN 201711320171 A CN201711320171 A CN 201711320171A CN 107915226 A CN107915226 A CN 107915226A
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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Abstract
The invention discloses a kind of preparation method and device of hydrogen-free absorbent charcoal material, method includes the following steps：Oxygen-containing gas is passed through into dielectric barrier discharge reactor, start to discharge after heating, then the hydrogen atoms activated carbon after screening is slowly sent into dielectric barrier discharge reactor, with the oxygen atom that electric discharge produces chemical reaction generation water occurs for the hydrogen atom of hydrogen atoms activated carbon surface, and hydrogen-free activated carbon is prepared.The method of the present invention is that the activated carbon of hydrogen atoms is placed in the space containing the oxygen after electric discharge, and chemical reaction generation water occurs for the hydrogen atom (being present in activated carbon surface in the form of carboxyl or hydroxyl) on the oxygen atom and activated carbon surface produced using electric discharge.
Description
Technical field
The technology of the present invention is related to a kind of preparation method and device with surface active ingredient activated carbon, particularly a kind of nothing
The preparation method and device of hydrogen activity charcoal.
Background technology
Now, activated carbon has been widely used in being permitted multicomponent absorption in air.Activated carbon is a kind of by processing
The porous material of processing.There is flourishing microcellular structure inside activated carbon, possess very big surface area, to some organic matters and nothing
Machine thing all has good adsorption capacity.There is an abundant group on the surface of activated carbon, including it is acid it is oxygen-containing contain hydrogen functional group, such as
Hydroxyl and carboxylic acid group.These hydrogeneous hydroxyls and carboxylic acid group hinder absorption of the oxygen to adsorbate in hydroxyl and carboxylic acid group, weaken
The binding ability between oxygen and adsorbate in hydroxyl and carboxylic acid group.Therefore there is an urgent need to develop one kind to contain a large amount of oxygen atoms but nothing
The activated carbon of hydrogen atom.
Activated carbon remodeling realized using water, as publication number CN106006632A Chinese invention patent application document in
2016.10.12 a kind of activated carbon modified device is disclosed, various functions base is loaded in activated carbon surface by vapor modification
Group, including acidic functionality (- COOH ,-OH ,-C=O) and basic functionality (- CH2,-CHR) Deng Shi activated carbon surfaces functional group
Change.
To increase the adsorption capacity of activated carbon, activated carbon surface can be handled using chemical method, be inhaled
Attached required functional group.For example, obtain adsorption capacity by increasing oxy radical.Open (bulletin) number CN10146204A
Chinese invention patent application document disclosed in 2009.06.24 and a kind of remove the activated carbon of thiophenes in gasoline and change
Property material and preparation, application process, the art solutions are higher to obtain using ozone as oxide isolation oxidation modification activated carbon
The active carbon adsorption material of Sulfur capacity.Activated carbon is subjected to deliming to activated carbon with the mixed acid of hydrochloric acid-hydrofluoric acid, uses deionized water
Washing is impregnated to neutrality, then with the sodium hydroxide solution of 1-4mol/L, loads reaction vessel after filtering, it is 5- to be passed through mass concentration
It is washed with deionized after the ozone-air mixed gas of 15mg/L to neutrality, is made after filtering, drying.
The report of hydrogen-free activated carbon is prepared there is presently no charging method.
The content of the invention
The present invention provides a kind of preparation method and device of hydrogen-free absorbent charcoal material, solves the problems, such as it is that exploitation one kind has
More preferable adsorption capacity and the activated carbon containing a large amount of oxygen atoms but without hydrogen atom of effect and more long-life.
A kind of preparation method of hydrogen-free absorbent charcoal material, includes the following steps：
(1) the hydrogen atoms activated carbon after sieving is through dehydration；
(2) oxygen-containing gas is passed through into dielectric barrier discharge reactor, starts to discharge after heating, then by after dehydration
Hydrogen atoms activated carbon be slowly sent into dielectric barrier discharge reactor, the hydrogen atom of hydrogen atoms activated carbon surface and electric discharge
Chemical reaction generation water occurs for the oxygen atom of generation, and hydrogen-free activated carbon is prepared.
Hydrogen-free activated carbon prepared by this method has the characteristics that adsorption capacity is high, activity is strong.First, in selection charcoal particle
Afterwards, the oxygen after being filled with electric discharge or gas (such as CO containing oxygen after electric discharge are just placed2, NO2) and other gases
(such as N2, He, Ar) gaseous mixture under conditions of handled.Electric discharge terminates, and is with activated carbon obtained after its natural cooling
For efficient hydrogen-free activated carbon.This activated carbon surface single contains oxygen atom group rich in substantial amounts of so that its adsorption capacity obtains
Great raising, service life are also extended.
The present invention carries out thermal dehydration processing after activated carbon to be processed is sieved, removing hydraulics are 120 DEG C of processing 1
~30min, then carries out oxygen discharge reaction again, makes the hydrogen atom Cheng Shui of activated carbon surface.
Involved chemical reaction is as follows.
After electric discharge, the hydrogen atom of traditional activated carbon surface is oxidized to water, and activated carbon surface contains largely can be with
Play the oxygen atom of suction-operated.The oxygen atom causes adsorption capacity to be significantly increased due to the presence of no hydrogen atom.
Preferably, the oxygen-containing gas gas is the mixed gas or purity oxygen of oxygenous gas and inert gas.
It is further preferred that oxygenous gas includes CO2With NO etc., the inert gas includes N2, He, Ar etc..
It is further preferred that the oxygen-containing gas is purity oxygen.
Discharge space gas temperature is 0-500 DEG C, it is preferable that is warming up to 50~120 after oxygen is passed through in discharge reactor
DEG C and 50~120 DEG C keep the temperature 20~40min after start to discharge.Heating can accelerate chemical reaction rate in advance, promote reaction
Reduce the time of catalyst preparation.
Whole discharge reactor can be placed in a high temperature furnace or discharge portion is placed on height by the control of temperature
In warm stove.
The absolute pressure of discharge space gas is 100Pa-10atm, it is preferable that the absolute pressure of gas in discharge reactor
For 50-200kPa.
Preferably, the reaction time of hydrogen atoms activated carbon and oxygen is 10~60min.Activated carbon is inside stainless steel tube
Processing time can be adjusted by discharging length of tube, can also be adjusted by the velocity of discharge of stainless steel tube active lower charcoal
Section.
Preferably, more than 95% particle diameter of hydrogen atoms activated carbon after screening is within the scope of 0.2mm-5mm.Further
Preferably, more than 95% particle diameter of hydrogen atoms activated carbon after screening is within the scope of 0.2mm-0.3mm.
Preferably, the flow that is passed through of oxygen is 200mL/min~400mL/min.It is further preferred that the involvement amount of oxygen
For 300mL/min.
Electric discharge mainly applies high voltage electric field using high voltage power supply to 2 metal electrodes, makes the gas discharge in discharge space,
The voltage waveform of high voltage power supply output can be alternating current and direct current or impulse form.
Preferably, dielectric barrier discharge reactor realizes that high voltage pulse peak value is 8~12kV using high-voltage pulse power source,
400~600Hz of pulse frequency.
It is further preferred that high voltage pulse peak value is 10kV, pulse frequency 500Hz.
The present invention also provides a kind of preparation facilities of hydrogen-free absorbent charcoal material, preparation method of the invention is preferably in the device
Middle progress, including the gas bomb and dielectric barrier discharge reactor being sequentially arranged, the dielectric barrier discharge reactor connection
High voltage power supply, the dielectric barrier discharge reactor include：
Metal pipe electrode, the metal tube electrode tube is interior to be sent into passage for activated carbon, and some gas passages are opened up on tube wall；
The block media protective case being sleeved on outside metal pipe electrode, forms envelope between block media protective case and metal pipe electrode
Space is closed to make gas discharge region, the gas discharge region is with the gas feed and metal for connecting the gas bomb
Connected in pipe electrode pipe by the gas passage；
And it is sleeved on the metal foil electrode outside block media protective case；
The metal pipe electrode connects the high voltage power supply with metal foil electrode.
Metal pipe electrode and metal foil electrode access the two poles of the earth that high voltage power supply connects high voltage power supply respectively, while metal foil
Electrode is grounded as grounding electrode.
Preferably, the metal pipe electrode is stainless steel tube electrode, and the metal foil electrode is stainless steel foil electrode, described
Dielectric impedance protective case is ceramics or glass protection sleeve.
Preferably, connect set on the pipeline of the gas bomb and the gas feed gas open-close valve, flowmeter and
Pressure gauge.Gas open-close valve, flowmeter and pressure gauge are sequentially arranged.
Electric discharge mainly applies high voltage electric field using high voltage power supply to 2 metal electrodes, makes the gas discharge in region of discharge,
The voltage waveform of high voltage power supply output can be alternating current and direct current or impulse form.
Preferably, the high voltage power supply is high-voltage pulse power source.
Preferably, the gas passage is the through hole being uniformly opened on stainless steel tube electrode tube wall.Plasma discharge
The gas containing oxygen atom produced afterwards is diffused in stainless steel tube by through hole, the atomic reaction of hydrogen with activated carbon surface.
It is further preferred that the through-hole diameter is 1~1.5mm, 2~4mm of centre distance between Kong Yukong.
Preferably, one end mouth of pipe of the stainless steel tube electrode is nothing to have hydrogen activity charcoal article inlet, the other end mouth of pipe
Hydrogen activity charcoal particle outlet.Have hydrogen activity charcoal particle from there is a hydrogen activity charcoal article inlet feeding, hydrogen-free activated carbon after reaction from
Hydrogen-free active carbon particle outlet output.
The method of the present invention is that the activated carbon of hydrogen atoms is placed in the space containing the oxygen after electric discharge, is produced using electric discharge
Chemistry occurs for the hydrogen atom (being present in activated carbon surface in the form of carboxyl or hydroxyl) on raw oxygen atom and activated carbon surface
Reaction generation water.
Apparatus of the present invention are made of basic a metal foil electrode, a glass or ceramic tube, a metal tube electrode
Unit preferably carries out in the apparatus of the present as dielectric barrier discharge reactor, method of the invention, glass or ceramic tube
Between metal foil electrode and metal pipe electrode.The gas compartment between glass or ceramic tube and metal pipe electrode is empty for electric discharge
Between, the gas in the space is provided by an extraneous gas import.There are a large amount of stomatas on metal tube electrode tube wall, can make discharging
Gas after the electric discharge of space enters inside metal tube.Active charcoal in space inside metal tube, activated carbon here will with put
The gas that electric space is come in reacts, and the hydrogen atom on activated carbon surface is oxidized to water.
It is of the invention with it is existing it is activated carbon modified compared with, have the following advantages that：
(1) present invention passes through modified method of discharging so that the various hydrogen atoms active groups of activated carbon surface are to list
One oxygen atom group that contains changes.It is this to show have pole than hydrogen atoms activated carbon in activated carbon surface containing oxygen atom group
Big adsorption capacity.
(2) adsorption capacity of the hydrogen-free Active Carbon in Organic obtained or inorganic matter is handled than hydrogeneous by the method for the present invention
Atom active charcoal is significantly increased.Such as the adsorption energy of the complicated organic matter such as complicated esters (such as isoamyl acetate), long-chain aldehyde
Power can improve 2-3 times；The adsorption capacity of hydrogen-free activated carbon PARA FORMALDEHYDE PRILLS(91,95) gas is 3-5 times of hydrogen atoms activated carbon.
(3) there is longer use compared to hydrogen atoms activated carbon by hydrogen-free activated carbon obtained by the method for the present invention
Service life.Such as the adsorption cleaning service life of Indoor Air Formaldehyde it is 5-6 times of hydrogen atoms activated carbon.
Brief description of the drawings
Fig. 1 is that the present invention always prepares reaction unit figure；
Fig. 2 is present media barrier discharge reactor schematic diagram；
Fig. 3 is that the formaldehyde adsorption property of hydrogen-free activated carbon and hydrogeneous activated carbon compares.
Reference numeral is as follows shown in Fig. 1 and Fig. 2：
1- gas bomb 2- gas switch valve 3- flowmeters
4- pressure gauge 5- high voltage power supply 6- dielectric barrier discharge reactors
61- oxygen-containing gas entrance 62- gas discharges region 63- metal pipe electrodes
64- metal foil electrode 65- gas passages 66- has hydrogen activity charcoal particle
67- hydrogen-free active carbon particles 68- has the outlet of hydrogen activity charcoal entrance 69- hydrogen-frees activated carbon
610- block media protective cases.
Embodiment
The technical solution in the embodiment of the present invention will be clearly and completely described below, protection scope of the present invention
It should not be limited by the examples, protection scope of the present invention is determined by claims.Based on the embodiments of the present invention, this area
Those of ordinary skill's all other embodiments obtained without creative efforts, belong to protection of the present invention
Scope.
As shown in Figure 1, a kind of device for preparing hydrogen-free activated carbon, including gas bomb 1 and dielectric barrier discharge reactor
6, connect and set gradually gas switch valve 2, flowmeter 3 and pressure on the pipeline of gas bomb and dielectric barrier discharge reactor
Table 4, dielectric barrier discharge reactor connection high voltage power supply 5, high voltage power supply is as ac high-voltage electric generator.
The sectional view of dielectric barrier discharge reactor is as shown in Fig. 2, including metal pipe electrode 63, metal foil electrode 64 and set
Block media protective case 610 between metal pipe electrode and metal foil electrode, metal pipe electrode use stainless steel tube electrode, no
Through hole is uniformly opened up on rust steel pipe tube wall as gas passage 65, one end mouth of pipe of stainless steel tube, which is used as, hydrogen activity charcoal entrance
68th, for the other end mouth of pipe as hydrogen-free activated carbon outlet 69, it is activated carbon passage that metal tube is interior.
Block media protective case is sleeved on outside stainless steel tube, is formed between stainless steel tube using ceramics or glass protection sleeve
Enclosure space, the enclosure space pass through as gas discharge region 62, gas discharge region with the activated carbon passage in metal tube
Gas passage 65 connects, set oxygen-containing gas import 61 on dielectric impedance protective case, import connection gas bomb.
Metal foil electrode uses stainless steel foil, is coated on outside block media protective case, metal pipe electrode and metal foil electrode
Access high voltage power supply 5 connects the two poles of the earth of high voltage power supply respectively, while metal foil electrode is grounded as grounding electrode.
Oxygen-containing gas is stored in gas bomb, is sent into by oxygen-containing gas import in gas discharge region, by exoelectrical reaction
Temperature in device starts to discharge after being increased to 50~120 DEG C of 20~40min of maintenance, then will have hydrogen activity charcoal particle 66 slowly to send
Enter in stainless steel tube, hydrogen atom (being present in activated carbon surface in the form of carboxyl or hydroxyl) and the electric discharge of activated carbon surface produce
Oxygen atom occur chemical reaction production water, hydrogen-free active carbon particle 67 is finally prepared.
Embodiment 1
First hydrogen atoms active carbon particle is sieved with the sieve that aperture is 0.3mm, then the sieve for being 0.2mm with aperture
Net sieves hydrogen atoms active carbon particle, and control hydrogen atoms active carbon particle size makes hydrogeneous in 0.2mm or so
Atom active charcoal ensures that more than 95% is within the scope of 0.2mm-0.3mm.
Oxygen (purity is not less than 99%) is passed through into discharge reactor, flow control is in 300mL/min.By exoelectrical reaction
Device is heated to 80 DEG C and starts to discharge after maintaining half an hour at 80 DEG C.
After starting electric discharge, the hydrogen atoms activated carbon filtered out (10 grams) is put into and is slowly added in discharge reactor.
Discharge reactor is 2 layers of pipe dielectric barrier discharge formula reactor, using the alumina ceramic tube (internal diameter of 2 millimeters thicks
500 millimeters of 20 mm outer diameter, 24 mm length) medium is done, thickness is that the stainless steel foil that 0.1 mm length is 400mm is wrapped in oxygen
Change and do electrode outside aluminum pipe, internal diameter is that 13 mm outer diameters are stainless steel tube that 15 mm lengths are 600 millimeters as electrode.Aluminium oxide
Tube top portion and bottom opening, stainless steel electrode are installed on inside alumina tube by the hole.Stainless steel electrode is in alumina tube
Aperture is uniformly opened in the region in portion, and hole diameter is 1 millimeter, 3 millimeters of the centre distance between Kong Yukong.One end of alumina tube is set
It is equipped with gas feed.Gases used is 100% oxygen.Stainless steel tube top is the inlet port of activated carbon to be processed, and lower part is
The outlet of activated carbon after processing.Whole discharge reactor can be placed in a high temperature furnace or discharge portion is placed on high temperature furnace
In.Processing time of the activated carbon inside stainless steel tube can be adjusted by discharging length of tube, can also pass through stainless steel tube
The velocity of discharge of active lower charcoal is adjusted.The discharge treatment time of this assay activity charcoal is 30 minutes.Electric discharge is to utilize height
The pulse power is pressed to realize.High voltage pulse peak value is 10kV, pulse frequency 500Hz.Treat that all activated carbons all pass through reactor
Stop heating afterwards, taken out after making the activated carbon Temperature fall room temperature after Dehydroepiandrosterone derivative, hydrogen-free activated carbon can be obtained.
Embodiment 2
It will be compared using hydrogen-free activated carbon made from the method for the present invention with traditional hydrogeneous activated carbon, formaldehyde absorbing purification is special
Property significantly improves.Fig. 3 is the relation curve of the concentration of formaldehyde and adsorption time after absorption.It can be seen that from the figure result
The hydrogen-free activated carbon that the method for the present invention obtains has larger adsorption capacity, and adsorption capacity is 3.7 times of hydrogeneous activated carbon, and formaldehyde is inhaled
Attached 4 times for reaching saturation time and being hydrogeneous activated carbon.
Claims (10)
1. a kind of preparation method of hydrogen-free absorbent charcoal material, it is characterised in that include the following steps：
(1) the hydrogen atoms activated carbon after sieving is through dehydration；
(2) oxygen-containing gas is passed through into dielectric barrier discharge reactor, starts to discharge after heating, then by containing after dehydration
Hydrogen atom activated carbon is slowly sent into dielectric barrier discharge reactor, and hydrogen atom and the electric discharge of hydrogen atoms activated carbon surface produce
Oxygen atom occur chemical reaction generation water, hydrogen-free activated carbon is prepared.
2. preparation method according to claim 1, it is characterised in that the oxygen-containing gas gas for oxygenous gas with it is lazy
The mixed gas or purity oxygen of property gas.
3. preparation method according to claim 1, it is characterised in that be passed through in discharge reactor after oxygen and be warming up to 50~
120 DEG C and 50~120 DEG C keep the temperature 20~40min after start to discharge.
4. preparation method according to claim 1, it is characterised in that the absolute pressure of gas is 50- in discharge reactor
200kPa。
5. preparation method according to claim 1, it is characterised in that the reaction time of hydrogen atoms activated carbon and oxygen is 10
~60min.
6. preparation method according to claim 1, it is characterised in that more than 95% particle diameter of hydrogen atoms activated carbon after screening
Within the scope of 0.2mm-5mm.
7. preparation method according to claim 1, it is characterised in that the flow that is passed through of oxygen is 200mL/min~400mL/
min。
8. preparation method according to claim 1, it is characterised in that dielectric barrier discharge reactor uses high-voltage pulse power source
Realize, high voltage pulse peak value is 8~12kV, 400~600Hz of pulse frequency.
9. a kind of preparation facilities of hydrogen-free absorbent charcoal material, including gas bomb and the dielectric barrier discharge reaction being sequentially arranged
Device, the dielectric barrier discharge reactor connect high voltage power supply, it is characterised in that the dielectric barrier discharge reactor includes：
Metal pipe electrode, the metal tube electrode tube is interior to be sent into passage for activated carbon, and some gas passages are opened up on tube wall；
The block media protective case being sleeved on outside metal pipe electrode, it is empty to form closing between block media protective case and metal pipe electrode
Between to make gas discharge region, the gas discharge region with connect the gas bomb gas feed, with metal tube electricity
Connected in pole pipe by the gas passage；
And it is sleeved on the metal foil electrode outside block media protective case；
The metal pipe electrode connects the high voltage power supply with metal foil electrode.
10. preparation facilities according to claim 9, it is characterised in that the metal pipe electrode is stainless steel tube electrode, described
Metal foil electrode is stainless steel foil electrode, and the dielectric impedance protective case is ceramics or glass protection sleeve.
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