CN107792855A - The removal methods of benzene in a kind of carbon dioxide - Google Patents
The removal methods of benzene in a kind of carbon dioxide Download PDFInfo
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- CN107792855A CN107792855A CN201610804957.0A CN201610804957A CN107792855A CN 107792855 A CN107792855 A CN 107792855A CN 201610804957 A CN201610804957 A CN 201610804957A CN 107792855 A CN107792855 A CN 107792855A
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- C01B2210/00—Purification or separation of specific gases
- C01B2210/0001—Separation or purification processing
- C01B2210/0003—Chemical processing
- C01B2210/0004—Chemical processing by oxidation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2210/00—Purification or separation of specific gases
- C01B2210/0001—Separation or purification processing
- C01B2210/0009—Physical processing
- C01B2210/0014—Physical processing by adsorption in solids
- C01B2210/0015—Physical processing by adsorption in solids characterised by the adsorbent
- C01B2210/0017—Carbon-based materials
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- C—CHEMISTRY; METALLURGY
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- C01B2210/00—Purification or separation of specific gases
- C01B2210/0043—Impurity removed
- C01B2210/0068—Organic compounds
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Abstract
The present invention relates to a kind of removal methods of benzene in carbon dioxide, including：Carbon dioxide containing benzene is mixed with background gas, forms pending mixed gas；The pending mixed gas is passed through catalyst reaction device, carries out reacting removing processing in the presence of a catalyst, obtains intermediate gas；And the intermediate gas is passed through adsorbent equipment, adsorbing and removing processing is carried out in the presence of adsorbent.Most benzene in carbon dioxide are reacted removing by the present invention by being catalyzed burning, then the benzene that adsorbing and removing remains on a small quantity, on the one hand realize the removing of benzene catalysis burning highly effective, another aspect adsorbing and removing can be carried out at normal temperatures, reduce energy expenditure, and higher purification requirement can be met, therefore the removing of benzene can be realized high efficiency, low cost.
Description
Technical field
The present invention relates to the field of purification of carbon dioxide, and in particular to the removing side of benzene in a kind of carbon dioxide
Method.
Background technology
Carbon dioxide belongs to ambient air greenhouse gases, and countries in the world are all restricted to CO2 emission, and China encourages
CO2 emission enterprise realizes that CO2 emission recycles.Food-class CO2It is the important addition of food service industry
Agent.However, the poisonous impurities such as some micro-benzenes can be contained in some carbon dioxide air sources, its recycling is limited.Benzene
Toxicity it is larger, Central nervous system has serious damaging effect, the particularly carbon dioxide as soda, to benzene
Content requirement is high.
At present, the administering method of waste gas containing benzene mainly has Production by Catalytic Combustion Process and absorption method etc..Production by Catalytic Combustion Process is organic matter
It is heated in the gas flow, under catalytic bed effect, accelerates organic-matter chemical reaction or the method for destroying efficiency.Catalyst is deposited
When making organic matter in heat damage, less retention time and lower temperature are needed than direct combustion method.Due to catalysis oxidation
Process is based only on the reaction of particular type compound, and high energy consumption, so the application of catalysis burning is restricted to a certain extent.
Also, food-class CO can not be realized using heat damage method sometimes2The purification requirement of high-purity.
Absorption method is utilized to the selective suction-operated of various impurity and to carbon dioxide weakly stable or non-adsorbable suction
The not volatile components contained in attached dose of removing source of the gas；The characteristics of absorption method is that whole adsorption-edulcoration processes are to be operated under normal temperature,
Recovery carbon dioxide process process is simple, energy consumption is low, and equipment is simple to operation, is widely favored.Adsorbent is for low dense
The poisonous impurities of degree can realize the purification of high-purity, but easily be reached for the source of the gas of high concentration poisonous impurities, adsorbent capacity
To saturation, it is necessary to could be come into operation again by frequently desorption, use cost is improved, also limit the extensive of this method
Using.
The content of the invention
In view of above-mentioned the deficiencies in the prior art, the present inventor proposes a kind of removal methods of benzene in carbon dioxide, leads to
Cross catalysis burning and the mode that is combined of adsorbing and removing, the benzene in carbon dioxide removal, energy consumption of reaction can be reduced, reduce purification
Cost；Meanwhile, it is capable to the dosage of adsorbent is saved, so as to efficiently, environmentally friendlyly realize the purification requirement of high-purity.
It is an object of the invention to provide a kind of removal methods of benzene in carbon dioxide, including：
Carbon dioxide containing benzene is mixed with background gas, forms pending mixed gas；
The pending mixed gas is passed through catalyst reaction device, carries out reacting at removing in the presence of a catalyst
Reason, obtains intermediate gas；And
The intermediate gas is passed through adsorbent equipment, carries out adsorbing and removing processing.
According to the present invention, by the carbon dioxide containing benzene and background gas be mixed to form pending mixed gas after,
It is passed through in catalyst reaction device, in the presence of a catalyst, the pending mixed gas is burnt and aoxidized, wherein the overwhelming majority
Benzene is oxidized to carbon dioxide, so as to which pending mixed gas is converted into what benzene concentration was greatly reduced by reacting removing processing
Intermediate gas, then, adsorbing and removing processing is carried out to the intermediate gas, remained with unreacted in adsorbing and removing intermediate gas
Benzene, so as to realize the further purification of carbon dioxide.
In the preferred embodiment of the present invention, in the background gas, the volume content of oxygen is 20-
30%, preferably 25%-30%, surplus are carbon dioxide.By the way that the carbon dioxide containing benzene and certain volume will be contained
The background gas of oxygen mix, and on the one hand can regulate and control the concentration of benzene in pending mixed gas, on the other hand, can ensure
Pending mixed gas has combustibility, can be sufficiently carried out catalytic oxidation.
In another preferred embodiment of the present invention, in the pending mixed gas, the gaseous mass of benzene is dense
Spend for 50-5000mg/m3, preferably 500-3000mg/L.
In another preferred embodiment of the present invention, the concentration of benzene is below 300mg/L in the intermediate gas,
Preferably below 200mg/L.The present inventor it has been investigated that, by the way that the concentration of benzene in intermediate gas is limited into above range
It is interior, catalyst combustion reaction can be made full use of to eliminate the benzene in pending mixed gas, so as to ensure the same of removal efficiency
When, the dosage of adsorbent has been saved, has reduced desorption frequency, has advantageously reduced purification cost.
In another preferred embodiment of the present invention, in the reaction removing processing, the pending gaseous mixture
The gas space velocity of body is 1000-20000h-1；Reaction temperature is 250 DEG C -300 DEG C.
In another preferred embodiment of the present invention, the temperature of the adsorbing and removing processing is 25-30 DEG C, the time
For 30-60min.
In another preferred embodiment of the present invention, the catalyst of the reaction removing processing is with selected from oxidation
At least one of aluminium, silica, titanium oxide, zinc oxide, calcium oxide are used as carrier, and are loaded with noble metal or base metal.
According to the present invention, above-mentioned urge can be prepared by by carrier impregnations such as aluminum oxide in containing noble metal or non-noble metal maceration extract
Agent.
In the preferred embodiment of the present invention, the carrier is aluminum oxide, and the noble metal is platinum or palladium,
The base metal is for copper and selected from least one of manganese, cerium, zirconium.
Noble metal catalyst is obtained with its excellent catalytic activity in VOCs (VOC) catalysis burnings
Extensive research and application.Compared with noble metal, the non-noble metal use cost such as copper is more cheap, and by with manganese, cerium,
Zirconium etc. is used in mixed way with rational proportioning, can also reach preferable catalytic effect.Also, due to the removal methods in the present invention
In, pending mixed gas will also carry out adsorbing and removing processing after catalysis is burnt, thus, from the sight for saving purification cost
Point sets out, preferably using the catalyst of base metal Supported alumina.
In the further preferred embodiment of the present invention, the base metal is included with copper, manganese, cerium and zirconium,
The copper, manganese, the mol ratio of cerium and zirconium are 1:1:1:0.1-1:1:1:1.
In another preferred embodiment of the present invention, the catalyst reaction device is to be filled with the catalyst
Shell-and-tube reactor or fixed-bed tube reactor, the adsorbent equipment include the adsorption treatment device of one or more series connection.According to
The degree of purification reached is needed, the adsorption treatment device of one or more series connection can be set.
In another preferred embodiment of the present invention, the adsorbent of adsorbing and removing processing be selected from activated carbon,
At least one of modified activated carbon, carbon molecular sieve and NACF, preferably modified activated carbon.
According to the present invention, by using porous carbon material as adsorbent, remained in adsorbing and removing intermediate gas
Benzene.It is similar with the structure of benzene because activated carbon has layered crystal structure, therefore be easier to adsorb than carbon molecular sieve etc.
Benzene.In the present invention, can be calcined by the way that fresh activity charcoal is added in the salpeter solution containing hydrogen peroxide after oxidation modification to prepare
Above-mentioned modified activated carbon.In the specific embodiment of the present invention, by fresh activity charcoal with 1g/100mL ratio, put
Enter mass fraction containing hydrogen peroxide in 10% salpeter solution, under normal temperature after stir about 3h, to be rinsed repeatedly to neutrality with deionized water,
Suction filtration obtains solid, and 105~110 DEG C of dryings 10~20 hours, are warming up to 145-150 DEG C of constant temperature 2h, are inhaled in Muffle furnace
Attached dose.
Preferably for benzene gaseous mass concentration below 1000mg/L pending mixed gas, due to using expensive
The removal effect difference of metallic catalyst and non-precious metal catalyst is little, from the viewpoint of cost-effective, preferably using non-
Noble metal catalyst.
Most benzene in carbon dioxide are reacted removing by the present invention by being catalyzed burning, and then adsorbing and removing is a small amount of
The benzene of residual, realize the removing of benzene with being on the one hand catalyzed burning highly effective so that into the gas of adsorbent equipment at benzene concentration
In relatively low level, benzene concentration is too high to exceed adsorption capacity so as to avoiding, and needs frequently to desorb repeatedly cumbersome, extends and sets
Standby usage time；Another aspect adsorbing and removing can be carried out at normal temperatures, reduce energy expenditure, and can meet higher purification
It is required that therefore the removing of benzene can be realized high efficiency, low cost.It should be noted that the removal methods of the present invention, which are removed, is applied to two
In carbonoxide outside the removing of benzene, the removing of benzene in other inert gases can be used for.
Brief description of the drawings
Fig. 1 be carbon dioxide provided by the invention in benzene removal methods schematic diagram (adsorbent equipment only containing one suction
The situation of attached processor).
Wherein, 1 is fixed-bed tube reactor, and 2 be the first adsorption tanks.
Fig. 2 is that (adsorbent equipment contains two series connection for the schematic diagram of removal methods of benzene in carbon dioxide provided by the invention
Adsorption treatment device situation).
Wherein, 1 is fixed-bed tube reactor, and 2 be the first adsorption tanks, and 3 be the second adsorption tanks.
Embodiment
The following example is only used for that the present invention is described in detail, it will be appreciated that the scope of the present invention is not limited to
These embodiments.
Embodiment 1
1) preparation of catalyst
Macropore boehmite, methylcellulose, soluble starch and acetic acid aqueous solution are mixed, kneading, are extruded into bar shaped.
In Muffle furnace under air atmosphere, 600 DEG C of maintenance 4h, Φ 3mm columns Al is obtained2O3Carrier.By column Al2O3Carrier is cut into 5mm
Long, incipient impregnation is in copper nitrate solution.Room temperature is put into Muffle furnace after drying, and is warming up in air atmosphere at 600 DEG C
4h is calcined, CuO/Al is made2O3Catalyst, it is designated as cat-1.
2) preparation of adsorbent
By fresh activity charcoal with 1g/100mL ratio, it is in 10% salpeter solution, often to be put into mass fraction containing hydrogen peroxide
After the lower stir about 3h of temperature, rinsed repeatedly with deionized water to neutrality, suction filtration and obtain solid, be placed in 110 DEG C of dryings 15 in Muffle furnace
Hour, constant temperature 2h is warming up to, obtains adsorbent.
3) removing is handled
Taking 2g cat-1, to be loaded into internal diameter be 0.7cm, in a length of 100cm quartz glass tube, is subsequently placed in fixed bed pipe
In formula reactor 1.2g adsorbent is taken to be put into the first adsorption tanks 2 and the second adsorption tanks 3 respectively, it is then anti-with fixed bed tubular type
Device 1 is answered to connect.
By background gas (carbon dioxide of the oxygen containing 25% volume content and 75% volume content) and pending benzene
Gas mixes by a certain percentage, to be configured to pending mixed gas of the gaseous mass concentration as 5000mg/L of benzene, then will
The mixed gas is passed through the gas set in fixed-bed tube reactor 1 in fixed-bed tube reactor 1 with 100ml/min flow velocity
Body air speed is 1500h-1, reaction temperature is 250 DEG C, carries out reacting removing processing.Complete reaction removing processing intermediate gas from
Fixed-bed tube reactor 1 passes sequentially through the first adsorption tanks 2 and the second adsorption tanks 3 after flowing out, and carries out adsorbing and removing at room temperature
Processing.
4) concentration mensuration
After starting to be passed through pending mixed gas 30min, using Agilent 7890A gas chromatographs respectively to fixed bed
The inlet and outlet a of tubular reactor 1, the outlet b of the first adsorption tanks 2 and the second adsorption tanks 3 outlet c benzene concentration are surveyed
Fixed, detector FID, chromatographic column is capillary column, and condition is column temperature：60 DEG C, fid detector：250℃.Measurement result is shown in
In table 1.
The removing processing to repeat the above steps 3), the difference is that only reaction temperature being arranged to 300 DEG C, carry out simultaneously
Concentration mensuration, measurement result are shown in Table 2.
The removing processing to repeat the above steps 3), the difference is that only and be arranged to the gaseous mass concentration of benzene
1000mg/L, while concentration mensuration is carried out, measurement result is shown in Table 3.
The removing processing to repeat the above steps 3), difference are that reaction temperature is arranged to 300 DEG C, and by the gas of benzene
Mass concentration is arranged to 1000mg/L, while carries out concentration mensuration, and measurement result is shown in Table 4.
Embodiment 2
1) preparation of catalyst
Macropore boehmite, methylcellulose, soluble starch and acetic acid aqueous solution are mixed, kneading, are extruded into bar shaped.
In Muffle furnace under air atmosphere, 600 DEG C of maintenance 4h, 3mm column alumina supports are obtained.In molar ratio 1:1:1:1, take nitric acid
Copper, manganese nitrate, cerous nitrate, each 1g of zirconium nitrate are added in deionized water, and heating obtains 100mL clarification mixed solutions, to oxidation
Aluminium carries out incipient impregnation 12h, filters after 140 DEG C in baking oven dry 12h, is finally putting into Muffle furnace and is calcined at 450 DEG C
4h, catalyst is obtained, be designated as cat-2.
Step 2) -4) carried out according to operation same as Example 1.
Embodiment 3
1) preparation of catalyst
Macropore boehmite, methylcellulose, soluble starch and acetic acid aqueous solution are mixed, kneading, are extruded into bar shaped.
In Muffle furnace under air atmosphere, 600 DEG C of maintenance 4h, 3mm column alumina supports are obtained.In molar ratio 1:1:1:0.5, take nitre
Sour copper 1g, manganese nitrate 1g, cerous nitrate 1g, zirconium nitrate 0.5g are added in deionized water, and it is molten that heating obtains 100mL clarification mixing
Liquid, incipient impregnation 12h is carried out to aluminum oxide, filters after 140 DEG C in baking oven dry 12h, is finally putting into Muffle furnace 450
4h is calcined at DEG C, obtains catalyst, is designated as cat-3.
Step 2) -4) carried out according to operation same as Example 1.
Embodiment 4
1) preparation of catalyst
Macropore boehmite, methylcellulose, soluble starch and acetic acid aqueous solution are mixed, kneading, are extruded into bar shaped.
In Muffle furnace under air atmosphere, 600 DEG C of maintenance 4h, 3mm column alumina supports are obtained.In molar ratio 1:1:1:0.1, take nitre
Sour copper 1g, manganese nitrate 1g, cerous nitrate 1g, zirconium nitrate 0.1g are added in deionized water, and it is molten that heating obtains 100mL clarification mixing
Liquid, incipient impregnation 12h is carried out to aluminum oxide, filters after 140 DEG C in baking oven dry 12h, is finally putting into Muffle furnace 450
4h is calcined at DEG C, obtains catalyst, is designated as cat-4.
Step 2) -4) carried out according to operation same as Example 1.
Embodiment 5
1) preparation of catalyst
By 1mgH2PtCl6It is dissolved in 2.5mL deionized waters, 0.5g meso-porous aluminas is impregnated in the solution, takes out true
After water in empty 12h removings system, with infrared light irradiation, and after carrying out reduction treatment with hydrazine hydrate, by sample in Muffle furnace
400 DEG C of annealing 2h, obtain the crystal hole wall mesoporous alumina catalyst material of the functionalization of Supported Pt Nanoparticles, the mass fraction of Supported Pt Nanoparticles
For 0.3%, cat-5 is designated as.
Step 2) -4) carried out according to operation same as Example 1.
Embodiment 6
1) preparation of catalyst
Meso-porous alumina is prepared with reference to embodiment 5.By 0.5mgH2PtCl6It is dissolved in 2.5mL deionized waters, by 0.5g oxygen
Change aluminium to be impregnated in the solution, after vacuumizing the water in 12h removing systems, with infrared light irradiation, and reduced with hydrazine hydrate
After processing, by sample, 400 DEG C of annealing 2h, the crystal hole wall meso-porous alumina for obtaining the functionalization of Supported Pt Nanoparticles are catalyzed in Muffle furnace
Agent material, the mass fraction of Supported Pt Nanoparticles is 0.1%, is designated as cat-6.
Step 2) -4) carried out according to operation same as Example 1.
Comparative example 1
2g adsorbent is taken to be put into the first adsorption tanks 2, by background gas (oxygen containing 25% volume content and 75% body
The carbon dioxide of product content) and pending benzene gas mix by a certain percentage, using be configured to the gaseous mass concentration of benzene as
5000mg/L pending mixed gas, the mixed gas is then passed through the first adsorption tanks 2 with 100ml/min flow velocity,
The adsorbing and removing processing of 1 hour is carried out at room temperature.After starting to be passed through pending mixed gas 30min, using Agilent 7890A
The gas chromatograph outlet b to the first adsorption tanks 2 under the same conditions as example 1 benzene concentration is measured, measure knot
Fruit is shown in Table 1.
Comparative example 2
According to the benzene concentration for the outlet b that the first adsorption tanks 2 are determined with the identical mode of comparative example 1, difference is to lead to
The gaseous mass concentration of benzene is 1000mg/L in the pending mixed gas entered, and measurement result is shown in Table 3.
Concentration (the mgL of benzene in 1 each exit gas of table-1)
| Outlet | cat-1 | cat-2 | cat-3 | cat-4 | cat-5 | cat-6 | Comparative example 1 |
| Export a | 509.2 | 417.3 | 315.0 | 322.0 | 283.5 | 231.4 | / |
| Export b | 52.9 | 47.4 | 38.7 | 29.1 | 27.6 | 22.3 | 4210.9 |
| Export c | 7.9 | 6.3 | 5.1 | 4.1 | 3.6 | 3.2 | / |
Remarks：The benzene concentration of entrance is 5000mgL-1。
Concentration (the mgL of benzene in 2 each exit gas of table-1)
| Outlet | cat-1 | cat-2 | cat-3 | cat-4 | cat-5 | cat-6 |
| Export a | 224.2 | 179.3 | 163.2 | 159.7 | 103.0 | 79.2 |
| Export b | 19.5 | 16.0 | 14.1 | 13.1 | 10.0 | 7.2 |
| Export c | 2.0 | 1.9 | 1.4 | 1.0 | 0.7 | 0.5 |
Remarks：The benzene concentration of entrance is 5000mgL-1。
Concentration (the mgL of benzene in 3 each exit gas of table-1)
| Outlet | cat-1 | cat-2 | cat-3 | cat-4 | cat-5 | cat-6 | Comparative example 2 |
| Export a | 27.2 | 15.4 | 17.5 | 17.9 | 11.1 | 10.8 | / |
| Export b | 4.2 | 1.7 | 2.3 | 2.3 | 0.8 | 0.8 | 322 |
| Export c | 0.1 | - | 0.1 | - | - | - | / |
Remarks：
1) benzene concentration of entrance is 1000mgL-1。
2) "/" is represented not detected, and "-" is represented because the concentration of benzene in detection gas is less than 0.1mgL-1, as a result show
It is shown as " not detecting ".
Concentration (the mgL of benzene in 3 each exit gas of table-1)
| Outlet | cat-1 | cat-2 | cat-3 | cat-4 | cat-5 | cat-6 |
| Export a | 14.3 | 9.8 | 13.2 | 12.9 | 7.2 | 6.3 |
| Export b | 2.1 | 0.8 | 2.3 | 2.3 | 0.7 | 0.6 |
| Export c | - | - | - | - | - | - |
1) benzene concentration of entrance is 1000mgL-1。
2) "-" is represented because the concentration of benzene in detection gas is less than 0.1mgL-1, as a result it is shown as " not detecting ".
It should be noted that embodiment described above is only used for explaining the present invention, do not form to any of the present invention
Limitation.By referring to exemplary embodiments, invention has been described, it should be appreciated that word wherein used is descriptive
With explanatory vocabulary, rather than limited vocabulary.The present invention can be made within the scope of the claims by regulation
Modification, and the present invention is revised in without departing substantially from scope and spirit of the present invention.Although the present invention described in it relates to
And specific method, material and embodiment, it is not intended that the present invention is limited to wherein disclosed particular case, on the contrary, this hair
It is bright to can be extended to other all methods and applications with identical function.
Claims (10)
1. the removal methods of benzene in a kind of carbon dioxide, including：
Carbon dioxide containing benzene is mixed with background gas, forms pending mixed gas；
The pending mixed gas is passed through catalyst reaction device, carries out reacting removing processing in the presence of a catalyst, obtains
To intermediate gas；And
The intermediate gas is passed through adsorbent equipment, adsorbing and removing processing is carried out in the presence of adsorbent.
2. removal methods according to claim 1, it is characterised in that in the background gas, the volume content of oxygen is
20-30%, preferably 25%-30%, surplus are carbon dioxide.
3. removal methods according to claim 1 or 2, it is characterised in that in the pending mixed gas, the gas of benzene
Weight concentration is 50-5000mg/L, preferably 500-3000mg/L.
4. according to the removal methods any one of claim 1-3, it is characterised in that the concentration of benzene in the intermediate gas
For below 300mg/L, preferably below 20mg/L.
5. according to the removal methods any one of claim 1-4, it is characterised in that in the reaction removing processing, institute
The gas space velocity for stating pending mixed gas is 1000-20000h-1；Reaction temperature is 250 DEG C -300 DEG C.
6. according to the removal methods any one of claim 1-5, it is characterised in that the temperature of the adsorbing and removing processing
For 25-30 DEG C, time 30-60min.
7. according to the removal methods any one of claim 1-6, it is characterised in that the catalysis of the reaction removing processing
Agent selected from least one of aluminum oxide, silica, titanium oxide, zinc oxide, calcium oxide, as carrier, and to be loaded with noble metal
Or base metal.
8. removal methods according to claim 7, it is characterised in that the carrier is aluminum oxide, and the noble metal is platinum
Or palladium, the base metal is for copper and selected from least one of manganese, cerium, zirconium.
9. according to the removal methods any one of claim 1-8, it is characterised in that the catalyst reaction device is filling
There are the shell-and-tube reactor or fixed-bed tube reactor of the catalyst, the adsorbent equipment includes the suction of one or more series connection
Attached processor.
10. according to the removal methods any one of claim 1-9, it is characterised in that the suction of the adsorbing and removing processing
Attached dose selected from least one of activated carbon, modified activated carbon, carbon molecular sieve and NACF.
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Application publication date: 20180313 |