CN104815614A - Preparation method of supported ferric activated carbons as well as condition and device applying supported ferric activated carbons to absorb methylbenzene - Google Patents
Preparation method of supported ferric activated carbons as well as condition and device applying supported ferric activated carbons to absorb methylbenzene Download PDFInfo
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Abstract
The invention discloses a preparation method of supported ferric activated carbons as well as a condition and a device applying the supported ferric activated carbons to absorb methylbenzene. The preparation method comprises the following steps: (1) preparing impregnation liquid: dissolving the weighed ferric salt into 0.1-10mol/L of acid solution, and preparing a mixed solution into the maceration extract at 20-80 DEG C; (2) impregnating active carbons: dipping the active carbons of which the granularity is 150-1700 [mu]m into the above impregnation liquid by adopting either an equivalent-volume impregnation method or an excessive impregnation method, wherein the mass ratio of the impregnated ferric elements and the active carbons is 0.025-0.35; (3) impregnating: placing the solution impregnated with the active carbons for 3-15 hours at room temperature; (4) drying: placing the impregnated active carbons into nitrogen at 150 DEG C to dry for 4-8 h, so as to obtain the supported ferric activated carbon. According to the preparation method of the supported ferric activated carbons provided by the invention, the metal element iron is impregnated to the active carbons to prepare the supported ferric activated carbons, therefore the absorption capacity of the active carbons can be improved, and the saturated adsorbing capacity of methylbenzene can be improved by 30-100%.
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 iron 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 stop using, the organic matter after absorption reclaims 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 iron 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 iron active carbon, comprises the steps:
(1) maceration extract is prepared: by load weighted iron salt dissolved 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, the active carbon of granularity 150 μm ~ 1700 μm be impregnated in above-mentioned maceration extract, after dipping, the mass ratio of ferro element and active carbon is 0.025 ~ 0.35;
(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 an iron active carbon.
Wherein, the molysite in described step (1) is one or more mixing in iron chloride, ferric nitrate, ferric sulfate, ferric acetate, ferric oxalate;
Acid solution is the hydrochloric acid solution of 1mol/L.
Wherein, the infusion process in described step (2) is the one in equi-volume impregnating and excessive infusion process.
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 iron and active carbon is 0.2 ~ 0.3;
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 iron 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 iron 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 iron 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 iron charcoal absorption toluene also comprises programmed temperature control instrument, and it is connected with described heating furnace.
The above-mentioned device carrying iron 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 iron 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 iron 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 iron 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 iron ion, 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 elements of ferrum impregnated on active carbon by the present invention, makes and carries iron active carbon, improves the adsorption capacity of active carbon, can improve 30% ~ 100% to the saturated extent of adsorption of toluene.
Accompanying drawing explanation
Fig. 1 is the structural representation utilizing the device carrying iron 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 iron active carbon, comprises the steps:
(1) maceration extract is prepared: by load weighted iron salt dissolved in the acid solution of 0.1 ~ 10mol/L, at the temperature of 20 ~ 80 DEG C, be mixed with maceration extract;
Wherein, molysite is one or more mixing in iron chloride, ferric nitrate, ferric sulfate, ferric acetate, ferric oxalate, preferred iron chloride.
The hydrochloric acid solution of acid solution preferably 1mol/L.
(2) Immesion active carbon: adopt equi-volume impregnating or excessive infusion process, the active carbon of granularity 150 μm ~ 1700 μm be impregnated in above-mentioned maceration extract, after dipping, the mass ratio of ferro element and active carbon is 0.025 ~ 0.35;
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 iron and active carbon is 0.2 ~ 0.3.
(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 an iron active carbon.
The present invention also provides a kind of and utilizes the above-mentioned adsorption conditions carrying iron 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 iron 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 iron 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 iron 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 iron 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), iron 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 iron and active carbon is respectively 0.028:1,0.056:1,0.084:1,0.112:1,0.224:1,0.336:1, 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
4, AC
5and AC
6.
By AC
0, AC
1, AC
2, AC
3, AC
4, AC
5and AC
6all 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 iron 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 | AC 6 |
| 200 | 60.05 | 103.42 | 95.65 | 99.87 | 108.43 | 109.24 | 103.67 |
| 160 | 76.07 | 126.77 | 118.53 | 122.47 | 127.89 | 132.39 | 131.52 |
| 120 | 95.12 | 149.46 | 137.93 | 142.88 | 150.13 | 159.01 | 152.41 |
| 80 | 125.28 | 169.47 | 156.65 | 166.94 | 169.59 | 184.16 | 177.17 |
| 40 | 157.01 | 204.83 | 192.00 | 202.66 | 206.43 | 226.32 | 217.40 |
From table 1 and Fig. 2, under identical adsorption conditions, the adsorbance that iron active carbon compares unmodified active carbon of carrying of different loads amount all has raising in various degree, and increase rate is 30% ~ 100%.
Embodiment two: iron 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 iron and active carbon is 0.05:1, 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 0.8MPa, gas flow 250mL/min, adsorption temp is 80 DEG C, the saturated extent of adsorption of toluene reaches 190.4mg/g active carbon, than the adsorbance 131.54 mg/g active carbon of active carbon unmodified under the same terms, improves 44.75%.
Embodiment three: iron 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 iron and active carbon is 0.34:1, 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 0.7MPa, gas flow 300mL/min, adsorption temp is 160 DEG C, the saturated extent of adsorption of toluene reaches 133.53mg/g active carbon, than the adsorbance 78.13 mg/g active carbon of active carbon unmodified under the same terms, improves 70.91%.
Embodiment four: iron 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 iron 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 0.3MPa, gas flow 250mL/min, adsorption temp is 200 DEG C, the saturated extent of adsorption of toluene reaches 112.5mg/g active carbon, than the adsorbance 60.9 mg/g active carbon of active carbon unmodified under the same terms, improves 84.73%.
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 iron 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 iron chloride is transformed to other molysite, adopts the preparation method in the present invention to prepare the modified activated carbon of load iron element, also should be considered as protection scope of the present invention.
Claims (10)
1. carry a preparation method for iron active carbon, it is characterized in that, comprise the steps:
(1) maceration extract is prepared: by load weighted iron salt dissolved 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, the active carbon of granularity 150 μm ~ 1700 μm be impregnated in above-mentioned maceration extract, after dipping, the mass ratio of ferro element and active carbon is 0.025 ~ 0.35;
(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 an iron active carbon.
2. the preparation method of according to claim 1 year iron active carbon, is characterized in that, the molysite in described step (1) is one or more mixing in iron chloride, ferric nitrate, ferric sulfate, ferric acetate, ferric oxalate;
Acid solution is the hydrochloric acid solution of 1mol/L.
3. the preparation method of according to claim 1 year iron active carbon, is characterized in that, the infusion process in described step (2) is the one in equi-volume impregnating and excessive infusion process.
4. the preparation method of according to claim 1 year iron 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 iron active carbon, is characterized in that, in described step (2), after dipping, the mass ratio of iron and active carbon is 0.2 ~ 0.3;
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 iron 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 iron 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 iron 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 iron 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 iron 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 iron 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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