CN104801272A - Preparation method of cobalt-supported activated carbon as well as condition and device for adsorbing methylbenzene with cobalt-supported activated carbon - Google Patents
Preparation method of cobalt-supported activated carbon as well as condition and device for adsorbing methylbenzene with cobalt-supported activated carbon Download PDFInfo
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Abstract
The invention discloses a preparation method of cobalt-supported activated carbon as well as a condition and a device for adsorbing methylbenzene with the cobalt-supported activated carbon. The preparation method comprises steps as follows: (1), preparation of a steeping liquor: weighed cobalt salt is dissolved into an acid solution with the specification of 0.1-10 mol/L, and the steeping liquor is prepared at the temperature of 20 DEG C-80 DEG C; (2), steeping of activated carbon: the activated carbon with the granularity being 10 meshes-100 meshes is steeped in the steeping liquor with an isometric steeping method or an excessive steeping method, and the mass ratio of cobalt to the activated carbon is 0.06-0.3 after steeping; (3), steeping: a solution for steeping the activated carbon is left to stand for 3-15 hours at a room temperature; (4) drying: the steeped activated carbon is put in nitrogen at the temperature of 150 DEG C and dried for 4-8 hours, and then the cobalt-supported activated carbon is acquired. The activated carbon is steeped in a solution containing the metal element cobalt, so that the cobalt-supported activated carbon is prepared, the adsorption capacity of the activated carbon is improved, and the saturation adsorption capacity for methylbenzene can be improved by 20%-110%.
Description
Technical field
The invention belongs to sorbing material and atmosphere pollution processing technology field, be specifically related to the preparation method of a kind of year cobalt active carbon and adsorb condition and the device of toluene with it.
Background technology
Along with the fast development of modern industry, the organic solvents such as the aromatic series such as carrene, toluene, dimethylbenzene, benzene, halogenated hydrocarbons, aldoketones, ester class, alcohols are widely used in the every field such as chemical industry, petrochemical industry, coating, medicine, rubber, resin, printing.These volatile organic solvents have toxicity mostly, and wherein quite a few finally enters in air with the form of organic exhaust gas, causes air to be heavily polluted.If dealt with improperly, namely cause raw-material loss, again contaminated environment, more seriously to the infringement of human health.The pay attention to day by day of Environmental protection work, improving constantly atmospheric emission standard, makes the recycling of organic exhaust gas imperative.From the organic exhaust gas of industrial discharge, reclaim organic solvent, namely can reduce the pollution to environment, reclaim again precious resources.
At present, the domestic process recovery method for industrial organic exhaust gas mainly contains: heating power burning method, condensation method, absorption absorption method, wherein adsorbing absorption method is carry out adsorption cleaning with Activated Carbon toward VOCs-Containing Exhausts, be its essence is that the characteristic utilizing active carbon high strength to adsorb is adsorbed onto in active carbon also concentrated the organic solvent in waste gas, directly emptying through charcoal absorption purified gas, this is the process of an Adsorption Concentration, organic solvent is not disposed, and is a physical process.When the organic matter adsorbed reaches the adsorbance of regulation, then the organic matter after absorption is stopped using to reclaim after desorption.Adsorbent, after absorption is saturated, can be passed through reproducer, recycles.
The characterization of adsorption of active carbon depends on the pore structure of its prosperity and unique surface chemical property.For the absorption property how improving active carbon, researcher starts with from the preparation of new carbon and normal activated carbon modification two aspect, achieves a series of achievement in research.The new carbon being used in adsorbing domain mainly refers to NACF, but its preparation process is often very complicated loaded down with trivial details, and cost is also far above normal activated carbon, and service condition is harsher.Above-mentioned shortcoming constrains NACF widely using in the industry.At present, the industrial material with carbon element for gas removal remains normal activated carbon.
At present, carried active carbon has been used to other systems such as desulfurization or separating ethene-ethane, but not yet for adsorbing toluene system, for the many employings of the adsorbing and removing of toluene in gas is the active carbon of non-carried metal, as Chinese invention patent 03159299.6 provides a kind of method for recovering toluene from exhausted air, toluene recovery rate can reach 65%, the toluene level < 40mg/m of the purified gas after purification
3, reach GB secondary standard.At normal temperatures, the saturated extent of adsorption of active carbon can meet general adsorption entails, but at high temperature the adsorbance of active carbon is very little.
Summary of the invention
The object of the invention is to provide the preparation method of a kind of year cobalt active carbon and adsorbs condition and the device of toluene with it.
For achieving the above object, the technical solution used in the present invention is: the preparation method of a kind of year cobalt active carbon, comprises the steps:
(1) maceration extract is prepared: by load weighted salt solubility in the acid solution of 0.1 ~ 10mol/L, at the temperature of 20 ~ 80 DEG C, be mixed with maceration extract;
(2) Immesion active carbon: adopt infusion process, granularity 10 order ~ 100 object active carbon be impregnated in above-mentioned maceration extract, after dipping, the mass ratio of cobalt element and active carbon is 0.06 ~ 0.3;
(3) flood: the solution after Immesion active carbon is put 3 ~ 15 hours in ambient temperatare;
(4) dry: the active carbon after dipping to be positioned in 150 DEG C of nitrogen dry 4 ~ 8 hours, obtains carrying a cobalt active carbon.
Wherein, the cobalt salt in described step (1) is one or more mixing in cobalt chloride, cobalt nitrate, cobaltous sulfate, cobalt acetate, cobalt oxalate;
Infusion process in described step (2) is the one in equi-volume impregnating and excessive infusion process.
Further, the cobalt salt in described step (1) is CoCL2 6H2O (CoC
l26H
2o), acid solution is the hydrochloric acid solution of 1mol/L.
Wherein, the active carbon in described step (2) is wooden, ature of coal, shell or coconut husk granular activated carbon.
Wherein, in described step (2), after dipping, the mass ratio of cobalt and active carbon is 0.15 ~ 0.2;
In described step (3), dip time is 12h, if auxiliary with ultrasonic vibration in dipping process, dip time can shorten 2 ~ 5 hours.
The embodiment of the present invention also provides a kind of and utilizes the above-mentioned adsorption conditions carrying cobalt charcoal absorption toluene, for: toluene level < 8% in toluene source of the gas, adsorptive pressure 0 ~ 1MPa, gas flow < 400mL/min, adsorption temp 40 ~ 200 DEG C.
The embodiment of the present invention also provides a kind of and utilizes the above-mentioned device carrying cobalt charcoal absorption toluene, comprise nitrogen cylinder, pressure-reducing valve, toluene gasification installation, the first valve, the second valve, the 3rd valve, the first rotor flowmeter, the second spinner flowmeter, in establish the adsorption column, heating furnace, precision pressure gauge, the second Mini-adjustable valve and the six-way valve that carry cobalt active carbon;
Described adsorption column is located in heating furnace;
Described pressure-reducing valve is arranged on the pipeline of connection nitrogen cylinder and toluene gasification installation;
Described first valve and the first rotor flowmeter are set in turn on the pipeline of the air inlet being communicated with toluene gasification installation and adsorption column;
Described second valve is arranged in the air inlet duct of connection nitrogen cylinder and adsorption column;
Described 3rd valve is arranged on the pipeline of connection second valve and adsorption column outlet;
The air inlet place of adsorption column is located at by described precision pressure gauge;
The gas outlet of described adsorption column is provided with described second Mini-adjustable valve by one and is connected with six-way valve with the pipeline of the second spinner flowmeter, and purified gas is emptying after flowing through described six-way valve.
The above-mentioned device carrying cobalt charcoal absorption toluene also comprises programmed temperature control instrument, and it is connected with described heating furnace.
The above-mentioned device carrying cobalt charcoal absorption toluene also comprises the first Mini-adjustable valve, its be arranged at be connected with the air inlet of described adsorption column, for regenerating time on-line analysis tracheae.
The above-mentioned device carrying cobalt charcoal absorption toluene also comprises gas chromatograph, and purified gas, to pass into the hydrogen of described six-way valve for carrier gas, flows out to gas chromatograph from described six-way valve.
The above-mentioned device carrying cobalt charcoal absorption toluene comprises 3 paths, respectively:
(1) on-line analysis path during regeneration, pressure-reducing valve, the second valve, the 3rd valve and the first Mini-adjustable valve are opened, first valve and the second Mini-adjustable valve are closed, nitrogen is as sweep gas, flow into below adsorption column, top is flowed out, and the toluene replacement adsorbed on the sorbent out, desorption gas enters gas-chromatography on-line analysis.
(2) containing the purification path of toluene source of the gas, pressure-reducing valve, the first valve and the second Mini-adjustable valve are opened, second valve, the 3rd valve and the first Mini-adjustable valve are closed, normality is flow through with nitrogen cylinder the nitrogen come after liquid toluene gasifies in toluene gasification installation to mix, then purify the toluene in it via adsorption column, purified gas is emptying by six-way valve.
(3) adsorption effect inspection path, pressure-reducing valve, the first valve and the second Mini-adjustable valve are opened, second valve, the 3rd valve and the first Mini-adjustable valve are closed, normality is flow through with nitrogen cylinder the nitrogen come after liquid toluene gasifies in toluene gasification installation to mix, then the toluene in it is purified via adsorption column, purified gas is that carrier gas is admitted to gas chromatograph with hydrogen, and the chromatogram shown by gas chromatograph is to analyze the adsorption effect of adsorption column.
The theoretical foundation that cobalt charcoal absorption toluene is carried in the present invention's utilization is: in toluene, the conjugatedπbond of phenyl ring can overlap to form σ key with the outer s unoccupied orbital of cobalt ions, meanwhile, and the π of benzene
*the d Orbital Overlap of antibonding unoccupied orbital and metal forms π complex bonds.This π Absorptive complex wave active force is better than physisorption power.Therefore in some occasion, such as, under high temperature, when physisorption power is very weak, π Absorptive complex wave still can play a role, thus strengthens the adsorption capacity of adsorbent.And π Absorptive complex wave active force is weaker than chemisorption power, therefore the regeneration of adsorbent can be realized again very easily.
Because technique scheme is used, the present invention compared with prior art has following advantages:
Metallic element cobalt impregnated on active carbon by the present invention, makes and carries cobalt active carbon, improves the adsorption capacity of active carbon, can improve 20% ~ 110% to the saturated extent of adsorption of toluene.
Accompanying drawing explanation
Fig. 1 is the structural representation utilizing the device carrying cobalt charcoal absorption toluene in the present invention;
Fig. 2 is the characterization of adsorption comparison diagram of adsorbent of identical adsorption conditions in the embodiment of the present invention one, different loads amount.
Wherein: 1, nitrogen cylinder; 2, pressure-reducing valve; 3, toluene gasification installation; 4, the first valve; 5, the second valve; 6, the first rotor flowmeter; 7, the second spinner flowmeter; 8, adsorption column; 9, heating furnace; 10, programmed temperature control instrument; 11, precision pressure gauge; 12, the first Mini-adjustable valve; 13, the second Mini-adjustable valve; 14, gas chromatograph; 15, six-way valve; 16, the 3rd valve.
Detailed description of the invention
Below in conjunction with drawings and Examples, the invention will be further described:
A preparation method for year cobalt active carbon, comprises the steps:
(1) maceration extract is prepared: be dissolved in the hydrochloric acid solution of 1mol/L by load weighted CoCL2 6H2O (CoCl26H2O), at the temperature of 20 ~ 80 DEG C, be mixed with maceration extract;
(2) Immesion active carbon: adopt equi-volume impregnating or excessive infusion process, granularity 10 order ~ 100 object active carbon be impregnated in above-mentioned maceration extract, after dipping, the mass ratio of cobalt element and active carbon is 0.06 ~ 0.3;
Wherein, active carbon can select one or more mixing in wooden, ature of coal, shell and coconut husk granular activated carbon.After dipping, the mass ratio of the optimum of cobalt element and active carbon is 0.15 ~ 0.2.
(3) flood: the solution after Immesion active carbon is put 3 ~ 15 hours in ambient temperatare;
Wherein, optimum dip time is 12h, if auxiliary with ultrasonic vibration in dipping process, dip time can shorten 2 ~ 5 hours.
(4) dry: the active carbon after dipping to be positioned in 150 DEG C of nitrogen dry 4 ~ 8 hours, obtains carrying a cobalt active carbon.
The present invention also provides a kind of and utilizes the above-mentioned adsorption conditions carrying cobalt charcoal absorption toluene, for: toluene level < 8% in toluene source of the gas, adsorptive pressure 0 ~ 1MPa, gas flow < 400mL/min, adsorption temp 40 ~ 200 DEG C.
The present invention also provides a kind of and utilizes the above-mentioned device carrying cobalt charcoal absorption toluene, structure as shown in Figure 1, comprise nitrogen cylinder 1, pressure-reducing valve 2, toluene gasification installation 3, first valve 4, second valve 5, the first rotor flowmeter 6, second spinner flowmeter 7, in establish and carry the adsorption column 8 of cobalt active carbon, heating furnace 9, its programmed temperature control instrument 10 be connected with described heating furnace 9, precision pressure gauge 11, first Mini-adjustable valve 12, second Mini-adjustable valve 13, gas chromatograph 14, six-way valve 15 and the 3rd valve 16.
Described adsorption column is located in heating furnace.
Described pressure-reducing valve is arranged on the pipeline of connection nitrogen cylinder and toluene gasification installation.
Described first valve is set in turn on the pipeline of the air inlet being communicated with toluene gasification installation and adsorption column with the first rotor flowmeter.
Described second valve is arranged in the air inlet duct of connection nitrogen cylinder and adsorption column.
Described 3rd valve is arranged on the pipeline of connection second valve and adsorption column outlet;
The air inlet place of adsorption column is located at by described precision pressure gauge.
Described first Mini-adjustable valve be arranged at be connected with the air inlet of described adsorption column, for regenerating time on-line analysis tracheae.
The gas outlet of described adsorption column is provided with described second Mini-adjustable valve by one and is connected with six-way valve with the pipeline of the second spinner flowmeter, and purified gas is emptying after flowing through described six-way valve.
Purified gas, to pass into the hydrogen of described six-way valve for carrier gas, flows out to gas chromatograph from described six-way valve.
The above-mentioned device carrying cobalt charcoal absorption toluene comprises 3 paths, respectively:
(1) on-line analysis path during regeneration, pressure-reducing valve, the second valve, the 3rd valve and the first Mini-adjustable valve are opened, first valve and the second Mini-adjustable valve are closed, nitrogen is as sweep gas, flow into below adsorption column, top is flowed out, and the toluene replacement adsorbed on the sorbent out, desorption gas enters gas-chromatography on-line analysis.
(2) containing the purification path of toluene source of the gas, pressure-reducing valve, the first valve and the second Mini-adjustable valve are opened, second valve, the 3rd valve and the first Mini-adjustable valve are closed, normality is flow through with nitrogen cylinder the nitrogen come after liquid toluene gasifies in toluene gasification installation to mix, then purify the toluene in it via adsorption column, purified gas is emptying by six-way valve.
(3) adsorption effect inspection path, pressure-reducing valve, the first valve and the second Mini-adjustable valve are opened, second valve, the 3rd valve and the first Mini-adjustable valve are closed, normality is flow through with nitrogen cylinder the nitrogen come after liquid toluene gasifies in toluene gasification installation to mix, then the toluene in it is purified via adsorption column, purified gas is that carrier gas is admitted to gas chromatograph with hydrogen, and the chromatogram shown by gas chromatograph is to analyze the adsorption effect of adsorption column.
For illustrating that the adsorbance of the of the present invention year relative normal activated carbon of cobalt active carbon increases, be described with several embodiment below.
Embodiment one: (active carbon without load is designated as AC for 20 ~ 40 object cocoanut active charcoals
0), cobalt chloride is dissolved in the HCl solution of the 1mol/L of certain volume, then by AC
0dipping wherein.In dipping system, the mass ratio of cobalt and active carbon is respectively 0.059:1,0.118:1,0.177:1,0.236:1,0.295:1, and after ambient temperatare puts 12h, dry in 150 DEG C of nitrogen, gained acticarbon is designated as AC respectively
1, AC
2, AC
3, AC
4and AC
5.
By AC
0, AC
1, AC
2, AC
3, AC
4and AC
5all carry out the adsorption experiment of toluene, adsorption conditions is: in toluene source of the gas, toluene level is 5%, and adsorptive pressure is 0.2MPa, gas flow 250mL/min.
When identical adsorption conditions, different loads amount, carry cobalt active carbon to the adsorption capacity of toluene as shown in table 1 and Fig. 2.
Table 1: the characterization of adsorption of different loads amount adsorbent
| Temperature (DEG C) | AC 0 | AC 1 | AC 2 | AC 3 | AC 4 | AC 5 |
| 200 | 60.05 | 115.73 | 104.39 | 116.80 | 99.39 | 98.29 |
| 160 | 76.07 | 134.55 | 126.41 | 138.32 | 127.28 | 125.34 |
| 120 | 95.12 | 156.19 | 150.55 | 157.72 | 145.87 | 143.19 |
| 80 | 125.28 | 181.59 | 169.73 | 182.52 | 167.33 | 162.34 |
| 40 | 157.01 | 212.64 | 207.37 | 220.21 | 202.36 | 200.30 |
From table 1 and Fig. 2, under identical adsorption conditions, different loads amount carry adsorbance that cobalt active carbon compares unmodified active carbon all have raising in various degree, increase rate to be 20% ~
110%。
Embodiment two: cobalt chloride is dissolved in the HCl solution of the 1mol/L of certain volume, then flooded wherein by active carbon AC, in dipping system, the mass ratio of cobalt and active carbon is 0.062:1, after ambient temperatare puts 12h, dry in 150 DEG C of nitrogen, then carry out the adsorption experiment of toluene.
In toluene source of the gas, toluene level is 3%, and adsorptive pressure is 0.2MPa, gas flow 200mL/min, adsorption temp is 40 DEG C, the saturated extent of adsorption of toluene reaches 210.48mg/g active carbon, than the adsorbance 155.79 mg/g active carbon of active carbon unmodified under the same terms, improves 35.10%.
Embodiment three: cobalt chloride is dissolved in the HCl solution of the 1mol/L of certain volume, then flooded wherein by active carbon AC, in dipping system, the mass ratio of cobalt and active carbon is 0.3:1, after ambient temperatare puts 12h, dry in 150 DEG C of nitrogen, then carry out the adsorption experiment of toluene.
In toluene source of the gas, toluene level is 4%, and adsorptive pressure is 0.3MPa, gas flow 300mL/min, adsorption temp is 120 DEG C, the saturated extent of adsorption of toluene reaches 140.36mg/g active carbon, than the adsorbance 94.11 mg/g active carbon of active carbon unmodified under the same terms, improves 49.14%.
Embodiment four: cobalt chloride is dissolved in the HCl solution of the 1mol/L of certain volume, then flooded wherein by active carbon AC, in dipping system, the mass ratio of cobalt and active carbon is 0.25:1, after ambient temperatare puts 12h, dry in 150 DEG C of nitrogen, then carry out the adsorption experiment of toluene.
In toluene source of the gas, toluene level is 5%, and adsorptive pressure is 1.0MPa, gas flow 250mL/min, adsorption temp is 200 DEG C, the saturated extent of adsorption of toluene reaches 122.35mg/g active carbon, than the adsorbance 70.91 mg/g active carbon of unmodified active carbon, improves 72.54%.
The above embodiments two, three, four describe different adsorption conditions, different loads amount, and the saturated extent of adsorption carrying the relatively unmodified active carbon of cobalt active carbon all increases.
The above is the preferred embodiment of the present invention; should be understood that; for those skilled in the art; under the prerequisite not departing from principle of the present invention; some improvement or replacement can also be made; such as cobalt chloride is transformed to other cobalt salts, adopts the preparation method in the present invention to prepare metal cobalt loaded modified activated carbon, also should be considered as protection scope of the present invention.
Claims (10)
1. carry a preparation method for cobalt active carbon, it is characterized in that, comprise the steps:
(1) maceration extract is prepared: by load weighted salt solubility in the acid solution of 0.1 ~ 10mol/L, at the temperature of 20 ~ 80 DEG C, be mixed with maceration extract;
(2) Immesion active carbon: adopt infusion process, granularity 10 order ~ 100 object active carbon be impregnated in above-mentioned maceration extract, after dipping, the mass ratio of cobalt element and active carbon is 0.06 ~ 0.3;
(3) flood: the solution after Immesion active carbon is put 3 ~ 15 hours in ambient temperatare;
(4) dry: the active carbon after dipping to be positioned in 150 DEG C of nitrogen dry 4 ~ 8 hours, obtains carrying a cobalt active carbon.
2. the preparation method of according to claim 1 year cobalt active carbon, is characterized in that, the cobalt salt in described step (1) is one or more mixing in cobalt chloride, cobalt nitrate, cobaltous sulfate, cobalt acetate, cobalt oxalate;
Infusion process in described step (2) is the one in equi-volume impregnating and excessive infusion process.
3. the preparation method of according to claim 1 year cobalt active carbon, is characterized in that, the cobalt salt in described step (1) is CoCL2 6H2O, and acid solution is the hydrochloric acid solution of 1mol/L.
4. the preparation method of according to claim 1 year cobalt active carbon, is characterized in that, the active carbon in described step (2) is wooden, ature of coal, shell or coconut husk granular activated carbon.
5. the preparation method of according to claim 1 year cobalt active carbon, is characterized in that, in described step (2), after dipping, the mass ratio of cobalt and active carbon is 0.15 ~ 0.2;
In described step (3), dip time is 12h, if auxiliary with ultrasonic vibration in dipping process, dip time can shorten 2 ~ 5 hours.
6. one kind utilizes the adsorption conditions carrying cobalt charcoal absorption toluene according to any one of Claims 1 to 5, it is characterized in that, toluene level < 8% in toluene source of the gas, adsorptive pressure 0 ~ 1MPa, gas flow < 400mL/min, adsorption temp 40 ~ 200 DEG C.
7. one kind utilizes the device carrying cobalt charcoal absorption toluene according to any one of Claims 1 to 5, it is characterized in that, comprise nitrogen cylinder, pressure-reducing valve, toluene gasification installation, the first valve, the second valve, the 3rd valve, the first rotor flowmeter, the second spinner flowmeter, in establish and carry the adsorption column of cobalt active carbon, heating furnace, precision pressure gauge, the second Mini-adjustable valve and six-way valve;
Described adsorption column is located in heating furnace;
Described pressure-reducing valve is arranged on the pipeline of connection nitrogen cylinder and toluene gasification installation;
Described first valve and the first rotor flowmeter are set in turn on the pipeline of the air inlet being communicated with toluene gasification installation and adsorption column;
Described second valve is arranged in the air inlet duct of connection nitrogen cylinder and adsorption column;
Described 3rd valve is arranged on the pipeline of connection second valve and adsorption column outlet;
The air inlet place of adsorption column is located at by described precision pressure gauge;
The gas outlet of described adsorption column is provided with described second Mini-adjustable valve by one and is connected with six-way valve with the pipeline of the second spinner flowmeter, and purified gas is emptying after flowing through described six-way valve.
8. the device of according to claim 7 year cobalt charcoal absorption toluene, is characterized in that, also comprise programmed temperature control instrument, and it is connected with described heating furnace.
9. the device of according to claim 7 year cobalt charcoal absorption toluene, is characterized in that, also comprises the first Mini-adjustable valve, its be arranged at be connected with the air inlet of described adsorption column, for regenerating time on-line analysis tracheae.
10. the device of according to claim 7 year cobalt charcoal absorption toluene, is characterized in that, also comprise gas chromatograph, purified gas with the hydrogen passing into described six-way valve for carrier gas flows out to gas chromatograph from described six-way valve.
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Application publication date: 20150729 |