CN103721676A - Iodized activated carbon and preparation method and application thereof - Google Patents
Iodized activated carbon and preparation method and application thereof Download PDFInfo
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- CN103721676A CN103721676A CN201310722055.9A CN201310722055A CN103721676A CN 103721676 A CN103721676 A CN 103721676A CN 201310722055 A CN201310722055 A CN 201310722055A CN 103721676 A CN103721676 A CN 103721676A
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Abstract
The invention discloses iodized activated carbon and a preparation method and application thereof and belongs to the field of preparation of activated carbon. The preparation method for the iodized activated carbon comprises the steps of treating the activated carbon by a pickling treatment mode and iodizing the activated carbon by using an iodine compound. The application method of the iodized activated carbon comprises the steps of canning the iodized activated carbon into a hollow pipe, wherein the bottom and the top of the hollow pipe are not sealed; filling the front end and the rear end of the activated carbon with glass fiber cotton in order to prevent leakage of the iodized activated carbon, wherein a mutual isolation function is realized during filling of multiple sections of the activated carbon. Due to the adsorption performance of the activated carbon to mercury in smoke, a mercury adsorption pipe can be applied to smoke monitoring and has the same performance as that of a foreign imported adsorption pipe, and the cost is low; the adsorption performance of the adsorption pipe can meet a technical requirement of EPA30B. The technical method is simple, is easy to operate and is low in cost and is suitable for monitoring the mercury in the smoke of a fixed pollution source.
Description
Technical field
The present invention relates to a kind of iodate active carbon and preparation method thereof and application, particularly for adsorbing, gather the total gaseous mercury of flue gas, be applied in stationary source gas mercury monitoring equipment.
Background technology
Mercury united state classifies global contaminant as in United Nations Environment Programme (UNEP), has the attribute of cross-boarder pollution, has become one of environmental contaminants of global extensive concern.All there is mercury pollution problem in the U.S., Europe, Africa and Asia, the even lonely arctic is also subject to the threat of mercury pollution.
The discharge of mercury mainly comes from natural source and artificial source two parts, and wherein fossil fuel (being mainly coal) burning is the artificial topmost source to airborne release mercury, accounts for 45.6% of global mercury emission.Mercury has effumability, and in burning of coal process, the mercury in coal first at high temperature volatilizees, and changes into elemental mercury (Hg
0), along with the reduction of cigarette temperature, in gas phase, part element mercury is oxidized to oxidation state mercury (Hg by the chemical reaction that series of complex occurs
2+), another part mercury is adsorbed by fly ash granule, forms particle mercury (Hg
p), so the mercury that combustion process is discharged in atmosphere mainly exists with three kinds of forms: elemental mercury, oxidation state mercury and particle mercury.Present stage, China's energy mainly take thermal power generation as main, due to coal combustion, to the mercury discharging in atmosphere, was about 200t. therefore every year
The mercury that burning produces enters the motion along with atmosphere after atmosphere and causes large-scale mercury pollution, mercury in atmosphere can enter water body along with sleet, enter the mercury of water body after methylating, easily be accumulated in fish and take piscivorous animals in main food chain, then the digestive system that enters people causes mercury poisoning, conventionally be again " minamata disease ", case appears at Japan first.Mercury comprises and causes renal function decay the harm of human body, infringement nervous system etc., so in combustion process, mercury emissions is subject to paying close attention to more and more widely.China has also carried out clear and definite regulation to mercury control aspect environmental requirement, as < < atmosphere comprehensive discharge standard > > (GB16297-2012), the pollutant emission standard > > of < < thermal power plant have all made related request to mercury emissions concentration.The international mercury pact of the United Nations is about to go out in 2013 issuing and implementation, and each national capital must be to the customary corresponding responsibilities and obligations of global mercury emissions when the time comes.
In order effectively to control mercury in flue gas discharge, first must monitor existing stationary source mercury emissions concentration, the development of the monitoring technology of current domestic mercury contaminants discharge but relatively lags behind, no matter from technology to equipment, mainly rely on external introduction, wherein common with EPA30B method monitoring mercury in flue gas concentration of emission, the method be by adsorption tube sample and extraction or thermoanalysis technology in conjunction with lab analysis method, both can be used as reference method to being arranged on the Hg CEMS of coal-burning boiler and the relative accuracy of Hg STMS detects audit, also as standard method, the Hg of discharged from coal-fired boiler is carried out to conventional detection, validity and accuracy in order to ensure monitored data, the method adopts two-way Parallel Sampling.But the mercury adsorption tube use amount in EPA30B method is sample of every collection to be changed once, and one group of data of every test need 2 adsorption tubes, in order to meet sampling Quality Control requirement, same measuring point need to gather at least 3 group data, needs 6 adsorption tubes, and use amount is very large.Moreover mercury adsorption tube mainly depends on import at present, expensive, according to above-mentioned sampling request, each measuring point only adsorption tube expense just needs four or five thousand yuan, therefore how to develop a kind of in performance can with the mercury adsorption tube that external import adsorption tube compares favourably and cost is cheap, become problem demanding prompt solution, and active ingredient is active carbon in mercury adsorption tube, therefore be necessary to find a kind of modified activated carbon, to improve the absorption property of active carbon to mercury in flue gas, make mercury adsorption tube be applied to flue gas monitoring, in performance, can compare favourably with external import adsorption tube and cost cheap, the absorption property of adsorption tube meets the specification requirement of EPA30B.
Summary of the invention
1, the technical problem that invention solves
High for current mercury monitoring cost, the invention provides a kind of iodate active carbon and preparation method thereof and application, mercury in flue gas is possessed preparation method and the application of iodate active carbon and the corresponding iodate active carbon of larger adsorption capacity.
2, technical scheme
Described active carbon is to require the background concentration of mercury low (<10ng/g), and particle diameter is at 20～200 object active carbons.For improving iodate effect, to active carbon, adopt acidifying pre-treatment to remove some impurity.
Iodate method for preparation of active carbon is as follows:
1) pre-treatment: adopt pickling processes mode to remove the impurity in active carbon, increase the specific area of active carbon, strengthen absorption property, described pickling processes mode can select the salpeter solution of 0.1～2mol/L to soak 12～48h, then with distilled water, active carbon is washed, wash to water outlet pH5～7, active carbon is dried under 40 ℃～120 ℃ conditions;
2) iodate is processed: adopt Surgidine to carry out iodate out to active carbon.
Employing is with M
1(iodine): M
2(sodium iodide)=1:K, the mass ratio of (0.8≤K≤3), the mass percent concentration being configured containing iodine is that 0.01%～3% compound iodine solution carries out active carbon iodate processing, with the Adsorption of Mercury ability of enhanced activity charcoal.Active carbon and compound iodine solution are fully stirred after 30～120min, the active carbon of absorption iodine is dried under 40 ℃～100 ℃ conditions.
The application process of iodate active carbon of the present invention: iodate charcoal canister is contained in hollow tube, the material of hollow tube necessarily requires mercury without absorption, high temperature resistant, prevent in sampling process because absorption causes measure error, does not shut at hollow tube bottom and top, for avoiding the leakage of iodate active carbon, in active carbon front and back end, all first filled glass fiber is cotton, plays on the one hand the impurity such as the particle that filters in flue gas, flue dust, when filling multistage active carbon, play the effect of mutual isolation.
3, beneficial effect
A kind of iodate active carbon of the present invention and preparation method thereof and application, adopting active carbon with low cost is raw material, and active carbon is carried out, after acidification, utilizing HNO
3strong oxidizing property, produce a large amount of acidic-groups, kind and the quantity of the soda acid official functional group of adjustable activity carbon surface, its surface chemical property, pore distribution are modified, the impurity of having removed active carbon itself presents the pore passage structure of marshalling, hole is flourishing, has increased the specific area of active carbon.Adopt iodate processing mode further to process active carbon, make activated carbon surface adsorb quantitative iodine, iodine can generate by there is chemical reaction the object that mercuric iodixde reaches Adsorption of Mercury with mercury.This process is simple, easily operation, with low cost, is applicable to the monitoring of stationary source mercury in flue gas.
Accompanying drawing explanation
Fig. 1 is for to be filled in the design sketch in hollow tube by iodate active carbon.1-the first section; 2-the 2nd section;
Fig. 2 is hollow tube inner structure schematic diagram.3-iodate active carbon; 4-glass fibre cotton.
The specific embodiment
Embodiment 1
Broken dry active carbon, chooses particle diameter at the background concentration <10ng/g(ng of 20～200 orders, mercury nanogram) activated carbon granule standby.Take 10g activated carbon granule and be placed in beaker, add the salpeter solution 200ml of 0.1mol/L to soak activated carbon granule simultaneously, soak time is 24h, then with distilled water, the active carbon after soaking is washed, wash to water outlet pH be 6, active carbon is dried under 105 ℃ of conditions, standby.
Adopt the compound iodine solution containing the mass percent concentration 0.01% of iodine to carry out active carbon iodate processing, with the Adsorption of Mercury ability of enhanced activity charcoal, concrete operation step is as follows: the preparation of compound iodine solution: according to mass ratio, i.e. and M
1(iodine): M
2it is 0.01% compound iodine solution 250ml that the mass ratio of (sodium iodide)=1:0.8 is configured mass concentration, it is colourless active carbon being immersed in compound iodine solution and being stirred well to solution colour, then by distilled water washing 3 times for the active carbon of processing through iodate, put into 50 ℃ of drying in oven to constant weight.
The active carbon of iodate is prepared into mercury adsorption tube, and material requested and step are as follows:
Material: ten thousand/balance, weighing spoon, pan paper, glass tube, glass fibre cotton, iodate active carbon
Step: 1) take iodate active carbon 1.0000 ± 0.0050g2 part, filter fiber cotton 0.2000 ± 0.0050g3 part
2) the iodate active carbon 3 weighing up, filter fiber cotton 4 are filled in and in double glazing pipe, carried out fillingly, preparation flow is:
Filter fiber cotton → iodate active carbon → filter fiber cotton → iodate active carbon → filter fiber is cotton, being about to iodate charcoal canister is contained in hollow tube, the material of hollow tube necessarily requires mercury without absorption, high temperature resistant, does not shut at hollow tube bottom and top, for avoiding the leakage of iodate active carbon, in active carbon front and back end, all first fill filter fiber cotton, when filling multistage active carbon, play the effect of mutual isolation.Prepared rear effect and iodate active carbon has been filled in to the design sketch in hollow tube, the first section 1, the 2 section 2 as Fig. 1; Fig. 2 is hollow tube inner structure schematic diagram, and iodate active carbon 3 is housed, glass fibre cotton 4.
Embodiment 2
Broken dry active carbon, chooses particle diameter standby at 20～200 object activated carbon granules.Take 10g activated carbon granule and be placed in beaker, add the salpeter solution 200ml of 0.1mol/L to soak activated carbon granule simultaneously, soak time is 24h, then with distilled water, the active carbon after soaking is washed, wash to water outlet pH be 6, active carbon is dried under 105 ℃ of conditions, standby.
Adopt the compound iodine solution of the mass percent concentration 0.01% that contains iodine to carry out active carbon iodate processing, with the Adsorption of Mercury ability of enhanced activity charcoal, concrete operation step is as follows: the preparation of compound iodine solution: the preparation of compound iodine solution: according to M
1(iodine): M
2it is 0.01% compound iodine solution 250ml that the mass ratio of (sodium iodide)=1:1.5 is configured mass concentration, it is colourless active carbon being immersed in compound iodine solution and being stirred well to solution colour, then by distilled water washing 3 times for the active carbon of processing through iodate, put into 50 ℃ of drying in oven to constant weight.
The active carbon of iodate is prepared into mercury adsorption tube, and material requested and step are as follows:
Material: ten thousand/balance, weighing spoon, pan paper, glass tube, glass fibre cotton, iodate active carbon
Step: 1) take iodate active carbon 1.0000 ± 0.0050g2 part, glass fibre cotton 0.2000 ± 0.0050g3 part
2) the iodate active carbon, the glass fibre cotton that weigh up are filled in and in glass tube, carried out fillingly, preparation flow is
Glass fibre cotton → iodate active carbon → glass fibre cotton → iodate active carbon → glass fibre cotton, has prepared rear effect as shown in Figure 1.
Embodiment 3
Broken dry active carbon, chooses particle diameter standby at 20～200 object activated carbon granules.Take 10g activated carbon granule and be placed in beaker, add the salpeter solution 200ml of 0.1mol/L to soak activated carbon granule simultaneously, soak time is 24h, then with distilled water, the active carbon after soaking is washed, wash to water outlet pH be 6, active carbon is dried under 105 ℃ of conditions, standby.
Adopt the compound iodine solution of the mass percent concentration 0.01% that contains iodine to carry out active carbon iodate processing, with the Adsorption of Mercury ability of enhanced activity charcoal, concrete operation step is as follows: the preparation of compound iodine solution: the preparation of compound iodine solution: according to M
1(iodine): M
2it is 0.01% compound iodine solution 250ml that the mass ratio of (sodium iodide)=1:3 is configured mass concentration, it is colourless active carbon being immersed in compound iodine solution and being stirred well to solution colour, then by distilled water washing 3 times for the active carbon of processing through iodate, put into 50 ℃ of drying in oven to constant weight.
The active carbon of iodate is prepared into mercury adsorption tube, and material requested and step are as follows:
Material: ten thousand/balance, weighing spoon, pan paper, glass tube, glass fibre cotton, iodate active carbon
Step: 1) take iodate active carbon 1.0000 ± 0.0050g2 part, glass fibre cotton 0.2000 ± 0.0050g3 part
2) the iodate active carbon, the glass fibre cotton that weigh up are filled in and in glass tube, carried out fillingly, preparation flow is
Glass fibre cotton → iodate active carbon → glass fibre cotton → iodate active carbon → glass fibre cotton, has prepared rear effect as shown in Figure 1.
Embodiment 4
Broken dry active carbon, chooses particle diameter standby at 20～200 object activated carbon granules.Take 10g activated carbon granule and be placed in beaker, add the salpeter solution 200ml of 2mol/L to soak activated carbon granule simultaneously, soak time is 24h, then with distilled water, the active carbon after soaking is washed, wash to water outlet pH be 6, active carbon is dried under 105 ℃ of conditions, standby.
Adopt the compound iodine solution of the mass percent concentration 1.5% that contains iodine to carry out active carbon iodate processing, with the Adsorption of Mercury ability of enhanced activity charcoal, concrete operation step is as follows: the preparation of compound iodine solution: the preparation of compound iodine solution: according to M
1(iodine): M
2it is 1.5% compound iodine solution 250ml that the mass ratio of (sodium iodide)=1:1.5 is configured mass concentration, it is colourless active carbon being immersed in compound iodine solution and being stirred well to solution colour, then by distilled water washing 3 times for the active carbon of processing through iodate, put into 50 ℃ of drying in oven to constant weight.
The active carbon of iodate is prepared into mercury adsorption tube, and material requested and step are as follows:
Material: ten thousand/balance, weighing spoon, pan paper, glass tube, glass fibre cotton, iodate active carbon
Step: 1) take iodate active carbon 1.0000 ± 0.0050g2 part, glass fibre cotton 0.2000 ± 0.0050g3 part
2) the iodate active carbon, the glass fibre cotton that weigh up are filled in and in glass tube, carried out fillingly, preparation flow is
Glass fibre cotton → iodate active carbon → glass fibre cotton → iodate active carbon → glass fibre cotton, has prepared rear effect as shown in Figure 1.
Embodiment 5
Broken dry active carbon, chooses particle diameter standby at 20～200 object activated carbon granules.Take 10g activated carbon granule and be placed in beaker, add the salpeter solution 200ml of 1mol/L to soak activated carbon granule simultaneously, soak time is 12h, then with distilled water, the active carbon after soaking is washed, wash to water outlet pH be 7, active carbon is dried under 120 ℃ of conditions, standby.
Adopt the compound iodine solution of the mass percent concentration 3% that contains iodine to carry out active carbon iodate processing, with the Adsorption of Mercury ability of enhanced activity charcoal, concrete operation step is as follows: the preparation of compound iodine solution: according to M
1(iodine): M
2it is 3% compound iodine solution 250ml that the mass ratio of (sodium iodide)=1:1.5 is configured mass concentration, it is colourless active carbon being immersed in compound iodine solution and being stirred well to solution colour, then by distilled water washing 3 times for the active carbon of processing through iodate, put into 100 ℃ of drying in oven to constant weight.
Embodiment 6
Broken dry active carbon, chooses particle diameter standby at 20～200 object activated carbon granules.Take 10g activated carbon granule and be placed in beaker, add the salpeter solution 200ml of 1.2mol/L to soak activated carbon granule simultaneously, soak time is 48h, then with distilled water, the active carbon after soaking is washed, wash to water outlet pH be 5, active carbon is dried under 40 ℃ of conditions, standby.
The compound iodine solution of employing 1.5% carries out active carbon iodate processing, and with the Adsorption of Mercury ability of enhanced activity charcoal, concrete operation step is as follows: the preparation of compound iodine solution: according to M
1(iodine): M
2it is 1.5% compound iodine solution 250ml that the mass ratio of (sodium iodide)=1:1.6 is configured mass concentration, active carbon after entering step 1 and processing is immersed in compound iodine solution and is stirred well to solution colour is colourless, then by distilled water washing 3 times for the active carbon of processing through iodate, put into 80 ℃ of drying in oven to constant weight.
Embodiment 7
The mercury adsorption tube of embodiment 5 preparations (being called for short adsorption tube A) is applied to mercury content in Fire Monitoring chimney of electric plant inlet flue gas, and carries out parallel performance test with import mercury adsorption tube (being called for short adsorption tube B).According to EPA30B method, require to carry out two-way Parallel Sampling, a road sampling is carried out mercury adsorption and enrichment with adsorption tube A, and another road sampling is carried out mercury adsorption and enrichment with adsorption tube B.The PMS30B Portable sampling device that mercury sampler adopts Nanjing Essen Environment Technology Co., Ltd to produce, adopts mercury content in the adsorption tube after Lumex RA-915M+ & Pyro-915+ type mercury analyzer analytical sampling.
The gas mercury solid absorption method of announcing according to the EPA Method30B(EPA of Environmental Protection Agency) whether effective method requirement, weigh mercury monitored data, and main performance index has two of penetrance, collimations.
Penetrance refers to that Hg passes the penetrance of adsorption tube the 1st section (in the 2nd section, the quality of Hg accounts for the percentage of the quality of Hg in the 1st section).When the acceptable standard of 30B is Hg > 1 μ g/m3,10% of the≤the 1 section Hg quality; During the μ g/m3 of Hg concentration≤1,20% of the≤the 1 section Hg quality.
Collimation refers to the uniformity of pairing adsorption tube measurement Hg quality.When the acceptable standard of 30B is Hg concentration > 1 μ g/m3, relative deviation (RD)≤10%; During the μ g/m3 of Hg concentration≤1, RD≤20% or absolute error≤0.2 μ g/m3.
Following table is that two types of adsorption tubes are monitored mercury content test result in certain chimney of electric plant inlet flue gas:
From site testing data, utilize adsorption tube A penetrance prepared by iodate active carbon all lower than 10%, meet the specification requirement of EPA30B, can guarantee the validity of measurement data.Show with import adsorption tube B parallel testing, two types of adsorption tube Hg measured value uniformity are good, and relative deviation, lower than 10%, meets the requirement of EPA30B mercury sampling collimation.Therefore, adsorption tube A can compare favourably with import adsorption tube on mercury adsorption features.
Claims (7)
1. an iodate method for preparation of active carbon, the steps include:
(1) pre-treatment: adopt pickling processes mode to remove the impurity in active carbon, described pickling processes mode is soaked activated carbon granule 12～48h with the salpeter solution of 0.1～2mol/L, then with distilled water, active carbon is washed, wash to water outlet pH5～7, active carbon is dried under 40 ℃～120 ℃ conditions, standby;
(2) iodate is processed: the ratio that is 1:0.8-3 in iodine and sodium iodide mass ratio is configured the compound iodine solution that the mass percent concentration containing iodine is 0.01%～3%, and after fully being stirred, the active carbon after step 1 is processed and compound iodine solution washs, the active carbon of absorption iodine is dried under 40 ℃～100 ℃ conditions, obtain iodate active carbon.
2. the preparation method of iodate active carbon according to claim 1, is characterized in that, the background concentration <10ng/g that the activated carbon granule in described step 1 is mercury, and particle diameter is at 20～200 object active carbons.
3. the preparation method of iodate active carbon according to claim 1, is characterized in that, the compound iodine solution in described step 2 is configured for take ratio that iodine and sodium iodide mass ratio be 1:1.5 the compound iodine solution that the mass percent concentration containing iodine is 3%.
4. the preparation method of iodate active carbon according to claim 1, is characterized in that, the washing in described step 2 is about to the distilled water washing 3 times for active carbon of processing through iodate.
5. the preparation method of iodate active carbon according to claim 1, is characterized in that, the washing in described step 1 is washed active carbon with distilled water, wash to water outlet pH be 7.
6. according to the resulting iodate active carbon of preparation method described in claim 1-5 any one.
According to the preparation-obtained iodate activated carbon application of claim 1-5 any one preparation method in preparing mercury adsorption tube, the steps include: iodate charcoal canister to be contained in hollow tube, does not shut at hollow tube bottom and top, for avoiding the leakage of iodate active carbon, in active carbon front and back end, all first filled glass fiber is cotton.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105561924A (en) * | 2016-01-29 | 2016-05-11 | 北京市劳动保护科学研究所 | Preparation method and application of modified activated carbon adsorbing agent for mercury in flue gas and collection tube of modified activated carbon adsorbing agent |
| CN109953130A (en) * | 2017-12-14 | 2019-07-02 | 丰益(上海)生物技术研发中心有限公司 | A kind of heavy fragrant peanut oil product of low pollution object content and preparation method thereof |
| CN110404505A (en) * | 2018-04-27 | 2019-11-05 | 中国矿业大学(北京) | For measuring the preparation method and active carbon of the active carbon of gaseous mercury |
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