CN100406113C - Preparation method of carried active carbon - Google Patents
Preparation method of carried active carbon Download PDFInfo
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- CN100406113C CN100406113C CNB2005100475410A CN200510047541A CN100406113C CN 100406113 C CN100406113 C CN 100406113C CN B2005100475410 A CNB2005100475410 A CN B2005100475410A CN 200510047541 A CN200510047541 A CN 200510047541A CN 100406113 C CN100406113 C CN 100406113C
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Abstract
A carrying activated carbon used for desulfurizing natural gas, removing SO2 from fume, or cleaning waste gas is prepared from activated carbon as carrier and additive component through impregnation method to distribute the additive component on the surface of the most of arteries in activated carbon.
Description
Technical field
The present invention relates to a kind of preparation method of active carbon, particularly use the preparation method of a certain amount of interpolation composition activity of infusion process load charcoal.
Background technology
Carried active carbon is one of modified activated carbon of using always, is widely used in synthetic ammonia, petrochemical industry, electronics, metallurgy, fields such as industry system ammonia, viscose rayon industry and environment-friendly engineering.According to the difference of application target, the component of load is different, generally is in the metal component one or more, or metal component and nonmetallic ingredient be used, sometimes also some organic matters of load.
Disclose a kind of auto-vulcanization hydrogen, sulphur carbonoxide, carbon disulfide inversion absorption type desulfurizing agent and preparation as CN1095963A, the aqueous solution of active carbon and potassium, sodium salt and organic amine or ethanol, acetone soln branch are soaked or soak altogether, dry then, roasting is made.CN1135456A discloses a kind of refined active carbon desulfurizer and preparation, this desulfurizing agent is made up of metallic compound and granular active carbon that the 1-3 kind is selected from Na, K, Mg, Ca, Ba, Ti, V, Cr, Mo, W, Mn, Fe, Co, Ni, Cu, Zn, Cd, Hg, Pb, its preparation method is that the water soluble salt with metal loads on the active carbon through too soaking or soaking altogether, and dry then or activation forms.97109206.0 disclose a kind of double-function fine dechlorination, desulfurizing agent and preparation method, by the reactive metal copper of load on active carrier and the carrier, chromium or also have the compound of sodium to form.Its preparation method be carrier active carbon with being selected from a kind of soluble copper salt and a kind of solubility chromic salts, the mixed solution that perhaps also has NaOH or sodium carbonate to be made into soaks altogether or step impregnation, air-dry and oven dry after form.CN1225289A discloses a kind of high sulfur capacity maceration active carbon used as dry method desulfurizer, with method load alkali compounds and mass transfer promoter on active carbon of soaking or dividing stain altogether, the organic alcohol of mass transfer promoter, acid and organic acid Na salt.CN1324686A discloses a kind of refined active carbon desulfurizer and preparation that removes mercaptan and thioether, is made up of the oxide of Na, Cu, Si or salt and active carbon.Its preparation method is that the water soluble compound with above-mentioned element adds before active carbon forming, or loads on the active carbon through too soaking or soaking altogether, and drying and activation form then.
When above-mentioned prior art has infusion process load on active carbon to add component; dipping solution direct impregnation granular activated carbon; the component of load can not be distributed on all surfaces, duct of active carbon; particularly can not be evenly distributed on all surfaces, duct of active carbon, the performance of active carbon needs further to improve.
Summary of the invention
At the deficiencies in the prior art; the invention provides a kind of preparation method of carried active carbon; before dipping granular activated carbon is carried out preliminary treatment, further improve the serviceability of carried active carbon, the inventive method goes for the preparation process of various support type modified activated carbons.
Carried active carbon preparation process of the present invention may further comprise the steps:
(1) gets or prepare granular activated carbon;
(2) preparation dipping solution;
(3) granular activated carbon that is soaked in water, soaking temperature is 20～150 ℃, preferred 50～100 ℃, soak time is 0.1～70h, preferred 1～3h;
(4) granular activated carbon after being soaked in water floods with dipping solution;
(5) activate behind the dipping, obtain final support type modified activated carbon.
Activated carbon granule described in the above-mentioned steps (1) can various suitable commercially available prod, also can prepare as required, can add suitable auxiliary agent as required in preparation process.
Dipping solution described in the above-mentioned steps (2) can be selected the compound of required load component according to the conventional knowledge preparation in this area, and the aqueous solution or organic solution that compound concentration is suitable can be added the promotion component that needs in the solution.When needing the load various ingredients, can prepare dipping solution respectively and divide and soak, also can prepare mixed solution and soak altogether.The component of load is generally one or more in metallic compound and the organic matter, can determine that load capacity is determined as required, is generally 0.05%～40% of active carbon weight according to the requirement of using.The concentration of solution is according to required load capacity and select the character of compound to determine that according to this area general knowledge being generally weight concentration is 0.5%～50%.
Above-mentioned steps (3) is an inventive point of the present invention, and promptly granular activated carbon carries out the preliminary treatment of water logging bubble before dipping.Can soak granular activated carbon with normal-temperature water during operation, be warming up to temperature required then and the maintenance required time.Also can earlier water be risen to temperature requiredly, soak granular activated carbon then.Temperature can remain unchanged in the dipping process, also can adjust.Soaking more than 100 ℃ as needs, then can under certain pressure, carry out, but not need operation like this usually.
Step (4) can adopt conventional dipping method, soaks etc. as soaking altogether or dividing, and dipping temperature can be selected normal temperature, and the time of normal temperature dipping was generally 0.2～72 hour.But be preferably as follows the dipping method under higher temperature: with dipping solution impregnated granules active carbon 0.01～72 hour under 40～150 ℃ of conditions of temperature, preferred 60～110 ℃ of dipping temperature most preferably is 75～100 ℃, and dip time is preferably 0.1～20 hour.Can use normal temperature dipping solution impregnation granular activated carbon during operation, be warming up to temperature required then and the maintenance required time.Also can earlier dipping solution be risen to temperature required, impregnated granules active carbon then.Temperature can remain unchanged in the dipping process, also can adjust.Be preferably in dipping under the slight boiling condition.Flooding more than 100 ℃ as needs, then can under certain pressure, carry out, but not need operation like this usually.
The routine operation mode is adopted in the described activation of step (5), generally comprises drying and roasting, for the active carbon of the organic interpolation component of some loads, only needs drying steps.Drying was generally carried out 1～70 hour under normal temperature～180 ℃, and roasting was generally carried out 0.5～30 hour under 180～400 ℃ of inert gas environments.
Find that through lot of experiments the immersion condition in the carried active carbon preparation process has bigger influence to the performance of modified activated carbon, and do not have relevant introduction in the prior art, all adopt the operation of normal temperature direct impregnation.The inventive method water before dipping steeps the bubble preliminary treatment, particularly adopts the immersion preliminary treatment under the higher temperature, has realized increasing substantially the effect of carried active carbon serviceability.By research, that granular activated carbon is soaked the possible cause that preliminary treatment can improve the active carbon serviceability is as follows for water under higher temperature.Active carbon is a porous material, also is the stronger material of adsorption capacity simultaneously, has been full of air in the active carbon duct before impregnation process.When active carbon flooded in solution, air was closed in the duct, and because the high adsorption capacity of active carbon, so be difficult to get rid of during dipping clean.Because the existence of air, dipping solution can not be full of all ducts of active carbon (duct that air occupies), its result must be can not the required interpolation component of load on the surface in the active carbon duct that do not contact with dipping solution, promptly this part active carbon fails to obtain modification, active carbon fails to make full use of, and the serviceability of final active carbon must be affected.Even perhaps dipping solution can be full of the duct of active carbon, also need the very long time, owing in the active carbon duct, just charge into the part duct that former air occupies through the long period at dipping solution, solute in the solution (needing the component of interpolation) majority is attracted to the duct part of flowing through, when charging into the duct that former air occupies, its solute concentration reduces greatly, also can cause the inhomogeneous of carried active carbon character thus, and finally influences serviceability.The present invention is by the preliminary treatment that is soaked in water under higher temperatures, higher temperature helps being adsorbed on the desorb of adsorbed gas in the active carbon duct, behind the high-temperature water preliminary treatment certain hour, air in the active carbon can be got rid of substantially, flood the influence that does not just have absorbed air then, make final products character even, improve serviceability.Be used in addition and carry out dip operation under the higher temperature, further reduced of the influence of the interior absorbed air of active carbon, improved the transmission speed of solute, further promote the character uniformity and the serviceability of carried active carbon dipping process.
The specific embodiment
The inventive method goes for the process that the loaded modified component of various infusion processes prepares special typed active carbon, as the desulfurization processing of various material gas, the adsorption refining of civilian all gases, the desulfurization processing of sulphur-containing exhaust gas etc.Because the difference of application, the load component of selection can be different, comprise the inorganic substances of metallic element and nonmetalloid, also need some organic matters sometimes.Among element Li, the Na that is usually directed to, K, Ca, Mg, Ba, Cu, Zn, Si, Ti, V, Cr, Mo, W, Mn, Fe, Co, Ni, Cd, Hg, Pb, Pt, La, Re, Sn, Sb, P, the Al etc. one or more.
Be process and the effect that example specifies the inventive method with the refining active carbon of selexol process, the refining active carbon of exhuast gas desulfurization below.But the present invention program can be easy to be applied to other purposes acticarbon that needs to add with the infusion process load component.
Embodiment 1～4
Get 10gPb (NO
3)
2Be put in the beaker that 100ml water is housed, evenly stir and make its whole dissolvings.Getting granularity is the active carbon 50g of 3mm, soak certain hour in the fresh water of different temperatures, the temperature of embodiment 1～2 fresh water is 30 ℃, and the active carbon soak time is respectively 0.5h and 24h, the temperature of embodiment 3～4 used fresh waters is respectively 80 ℃ and 100 ℃, and the active carbon soak time is 1h.Active carbon behind the water logging bubble is put in the Pb (NO of preparation just now
3)
2In the solution, at Pb (NO
3)
2Behind dipping 24h under the room temperature, at room temperature airing is put into tube furnace with the active carbon of airing, feeds steam, is heated to 750 ℃ then, activation 10h.The amount of steam is 2～3 tons of/ton active carbons.
Comparative example 1
Pb (the NO that preparation is identical with embodiment 1～4
3)
2Solution, Immesion active carbon.Different with embodiment is, in the comparative example, is not soaked in water before the soaking solution, directly active carbon is soaked in the Pb (NO for preparing
3)
2In the solution, dipping 24h, at room temperature airing is put into tube furnace with the active carbon of airing, feeds steam, is heated to 750 ℃ then, activation 10h.The amount of steam is 2～3 tons of/ton active carbons.
Employing embodiment 1～4 prepared active carbon removes the sulfide in the natural gas, and the concentration of sulfide is 70～100 μ L/L in the natural gas, air speed 1500h
-1, temperature is a normal temperature, gained Sulfur capacity such as table 1.
Sulfur capacity when table 1 embodiment 1～4 different soaking temperatures remove sulfide in the natural gas
Embodiment 5～10
Get 10gNa
2CO
3Be dissolved in the beaker that 100ml water is housed, stirring makes its whole dissolvings.Getting granularity is the active carbon 50g of 3mm, soak certain hour in the fresh water of different temperatures, the temperature of embodiment 5～6 fresh waters is 50 ℃, and the active carbon soak time is respectively 1h and 36h, the temperature of embodiment 3～4 used fresh waters is respectively 90 ℃ and 120 ℃, and the active carbon soak time is 0.5h.Active carbon behind the water logging bubble is put in the Na of preparation just now
2CO
3In the solution, at 90 ℃ Na
2CO
3Flood 12h in the solution, feed 160 ℃ hot-air then, dry 10h, the amount of hot-air is 2000～3000 times of active carbon/h.
Comparative example 2
The Na that preparation is identical with embodiment 5～10
2CO
3Solution, Immesion active carbon.Different with embodiment is, in the comparative example, is not soaked in water before the soaking solution, directly active carbon is soaked in the Na for preparing 90 ℃
2CO
32In the solution, flood 12h, feed 160 ℃ hot-air then, dry 10h, the amount of hot-air is 2000～3000 times of active carbon/h.
Employing embodiment 5～10 prepared active carbons remove the SO in the power-plant flue gas
2, the SO in the flue gas
2Concentration be 3000～5000 μ L/L (volume ratio), air speed 1500h
-1, temperature is a normal temperature, SO
2Adsorbance such as table 2.
Sulfur capacity when table 2 embodiment 5～10 different soaking temperatures remove sulfur dioxide in flue gas
| Project | The fresh water temperature | Soak time, h | SO 2Adsorbance (wt%) |
| Embodiment 5 | 50 | 1 | 8.8 |
| Embodiment 6 | 50 | 36 | 12.1 |
| Embodiment 7 | 90 | 0.5 | 13.8 |
| Embodiment 8 | 120 | 0.5 | 16.5 |
| Comparative example 2 | - | - | 7.9 |
Embodiment 11～12
Get 6gKOH and 0.5g ethylenediamine and be dissolved in the beaker that 100ml water is housed, all after the dissolving, stir.Getting granularity is the active carbon 50g of 3mm, soaks certain hour in the fresh water of different temperatures, and the temperature of embodiment 11 fresh waters is 30 ℃, and the active carbon soak time is 1h, and the temperature of embodiment 12 used fresh waters is respectively 100 ℃, and the active carbon soak time is 1h.Active carbon behind the water logging bubble is put in the KOH solution of preparation just now, in 40 ℃ KOH solution, floods 2h, then dry 10h under 120 ℃ temperature.
Comparative example 3
The KOH solution that preparation is identical with embodiment 11～12, Immesion active carbon.Different with embodiment is, in the comparative example, is not soaked in water before the soaking solution, directly active carbon is soaked in the KOH solution for preparing 40 ℃ dipping 2h, dry 10h under 120 ℃ temperature then.
Employing embodiment 11～12 prepared active carbons remove the H in the waste gas
2S, H
2S concentration is 1000 μ L/L, air speed 1000h
-1, 3 couples of H of embodiment 11～12 and comparative example
2Adsorbance such as the table 3 of S.
Table 3 embodiment 11～12 different soaking temperatures remove H
2Sulfur capacity during S
| Project | The fresh water temperature | Soak time, h | H 2S penetrates Sulfur capacity (wt%) |
| Embodiment 11 | 40 | 1 | 18.3 |
| Embodiment 12 | 100 | 1 | 32.3 |
| Comparative example 3 | - | - | 8.3 |
Claims (10)
1. the preparation method of a carried active carbon may further comprise the steps:
(1) gets or prepare granular activated carbon;
(2) preparation dipping solution;
(3) granular activated carbon that is soaked in water, soaking temperature is 20～150 ℃, soak time is 0.1～70h;
(4) granular activated carbon after being soaked in water floods with dipping solution;
(5) activate behind the dipping, obtain final support type modified activated carbon.
2. in accordance with the method for claim 1, it is characterized in that described soaking temperature is 50～100 ℃, soak time 1～3h.
3. in accordance with the method for claim 2, soak granular activated carbon with normal-temperature water when it is characterized in that dip operation, be warming up to temperature required then and the maintenance required time; Or earlier water is risen to temperature requiredly, soak granular activated carbon then.
4. in accordance with the method for claim 1, it is characterized in that the described dipping solution of step (4) dipping adopts normal temperature dipping or floods under higher temperature.
5. in accordance with the method for claim 4, it is characterized in that described under higher temperature immersion condition be: the impregnated granules active carbon is 0.01～72 hour under 40～150 ℃ of conditions of temperature.
6. in accordance with the method for claim 5, it is characterized in that described dipping temperature is that 60～110 ℃ of dip times are preferably 0.1～20 hour.
7. in accordance with the method for claim 5, it is characterized in that described dipping temperature is 75～100 ℃.
8. in accordance with the method for claim 4, it is characterized in that described the dipping is with normal temperature dipping solution impregnation granular activated carbon under higher temperature, be warming up to temperature required then and the maintenance required time; Or earlier dipping solution is risen to temperature required, impregnated granules active carbon then.
9. in accordance with the method for claim 1, it is characterized in that the described activation of step (5) comprises drying and roasting,, only need drying steps for the active carbon of the organic interpolation component of some loads.
10. in accordance with the method for claim 9, it is characterized in that described drying carried out 1～70 hour under normal temperature～180 ℃, roasting was carried out 0.5～30 hour under 180～400 ℃ of inert gas environments.
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| CNB2005100475410A CN100406113C (en) | 2005-10-26 | 2005-10-26 | Preparation method of carried active carbon |
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|---|---|---|---|
| CNB2005100475410A CN100406113C (en) | 2005-10-26 | 2005-10-26 | Preparation method of carried active carbon |
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| CN100406113C true CN100406113C (en) | 2008-07-30 |
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| CN101811025A (en) * | 2010-04-20 | 2010-08-25 | 南京师范大学 | Adsorbent for methylbenzene desulfuration and preparation method thereof |
| CN103111290A (en) * | 2013-03-18 | 2013-05-22 | 哈尔滨工业大学 | Preparation method of catalyst for catalyzing ozonation for advanced treatment of coal chemical wastewater |
| CN108219830A (en) * | 2018-03-28 | 2018-06-29 | 山东星火科学技术研究院 | A kind of diesel oil desulphurization technology |
| CN114950471B (en) * | 2022-06-30 | 2023-07-25 | 东营科尔特新材料有限公司 | Nickel-based catalyst, preparation method thereof and application thereof in selective hydrogenation of acetylene in ethylene |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1186841A (en) * | 1998-01-21 | 1998-07-08 | 太原理工大学 | Organic sulphur eliminating agent with normal temperature modified active carbon and its preparation |
| CN1324686A (en) * | 2000-05-24 | 2001-12-05 | 湖北省化学研究所 | Refined active carbon desulfurizer for eliminating mercaptan and thioether and its prepn. |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1186841A (en) * | 1998-01-21 | 1998-07-08 | 太原理工大学 | Organic sulphur eliminating agent with normal temperature modified active carbon and its preparation |
| CN1324686A (en) * | 2000-05-24 | 2001-12-05 | 湖北省化学研究所 | Refined active carbon desulfurizer for eliminating mercaptan and thioether and its prepn. |
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