Background technology
Coal is the most widely used one in numerous energy, for instance in the power generation of China, and the electric power of nearly 70% is produced by coal fired power generation. Along with socioeconomic development, Chinese energy consumption presents the trend risen year by year.
In actual boiler fired coal process, due to the imperfect combustion of coal dust, unburned carbon (including carbon black granules and residual Jiao) can be formed, and be finally mingled in flying dust, both cause the waste of fuel, the pollution of atmospheric environment can be brought again. In unburned carbon, carbon black granules is the rich soot particulate matter of a kind of reunion shape superfine by the particle diameter formed by a series of complex reaction containing hydrocarbon gas precursor, and general diameter is less than 0.1 micron. Carbon black granules is difficult to be trapped by traditional dust arrester, once be discharged in air, namely becomes air PM2.5Important component part, environmental and human health impacts can be produced serious influence. Research shows, carbon black has strong extinction characteristic, is the second largest reason causing greenhouse effect. It addition, carbon black granules has extremely strong surface activity, it is possible to health is had by absorption air the pollutant of very big threat, such as carcinogenic, teratogenesis, mutagenic matter etc. Residual Jiao is pulverized coal particle imperfect combustion and the carbonaceous products that left behind, generally has loose structure, and diameter is more than 1 micron. In burned-coal fly ash, the existence of residual Jiao not only can reduce the transformation efficiency of coal, also can affect the serviceability of burned-coal fly ash, as when utilizing burned-coal fly ash to make cement, the higher meeting of phosphorus content causes that strength of cement declines, thus being unsatisfactory for demand of industrial production.
Traditional separation about carbon black granules in burned-coal fly ash and residual Jiao and quantitative approach rarely have report.Paul etc. (Fuel, 1987,66:210-215) report the burning using thermogravimetric analyzer to study residual Jiao, the existence of carbon black granules detected in experiment. But this method is only when the amount of carbon black granules is relatively larger, thermogravimetric analyzer just can have obvious signal; When the amount of carbon black granules is less, the signal of carbon black granules cannot be detected. And this method can not realize physical separation and the quantitative study of carbon black granules and residual Jiao. It addition, thermogravimetric analyzer price general charged is costly, mostly use in institution of higher learning and scientific research institution, less for using coal-burning power plant. (the CombustionandFlame such as Sadakata, 1984,56:245-249) propose the Submicron Particles (including carbon black granules) collecting in coal-fired process first by Andersen particulate matter ram, then use carbon in elemental analyser detection Submicron Particles, hydrogen content so that it is determined that the quality of carbon black granules. This method has bigger difficulty for actual coal-burning power plant, because it needs to use special sampling instrument that particulate matter is carried out isokinetic sampling, Andersen particulate matter ram is expensive on the one hand, sampling process is extremely complex on the other hand, personal error is relatively big, and residual Jiao in flying dust cannot be carried out detection by quantitative by this method.
Therefore, for assessing the utilizability of the impact on environment of the efficiency of combustion of coal dust, particulate matter of black carbon and burned-coal fly ash, it is highly desirable to the carbon black granules in burned-coal fly ash and residual Jiao are effectively separated and quantitative assay.
Summary of the invention
Based on this, it is necessary to provide separating and method for quantitatively determining of carbon black granules and residual Jiao in a kind of burned-coal fly ash.
In a kind of burned-coal fly ash, carbon black granules and the separation method of residual Jiao, comprise the steps:
Use liquid dispersant to disperse described burned-coal fly ash, and carry out ultrasonic vibration, obtain burned-coal fly ash suspension;
Standing described burned-coal fly ash suspension makes described residual Jiao precipitate, thus layering occur in described liquid dispersant in described carbon black granules and described residual Jiao, generates the precipitated phase mutually and containing described residual Jiao that floats containing described carbon black granules;
Collect described floating mutually and described precipitated phase respectively, namely realize separating carbon black granules in burned-coal fly ash and residual Jiao.
Wherein in an embodiment, described separation method also includes repeating the step separating and purifying respectively described carbon black granules and described residual Jiao, the described step separating and purifying respectively described carbon black granules and described residual Jiao that repeats specifically includes: continue to add described liquid dispersant in the described precipitated phase collected, and the floating respectively liquid dispersant containing described precipitated phase and back collected is sequentially carried out ultrasonic vibration mutually and standing processes, then collect respectively stand after the floating phase of layering and precipitated phase.
Wherein in an embodiment, described in repeat separation and purify described carbon black granules and described residual Jiao respectively till described floating does not have precipitated phase appearance after ultrasonic vibration and standing process.
Wherein in an embodiment, described liquid dispersant is at least one liquid in water, methanol, ethanol and ethylene glycol.
Wherein in an embodiment, the power of described ultrasonic vibration is 0.1��0.5kW.
In above-mentioned burned-coal fly ash, carbon black granules in burned-coal fly ash and residual Jiao can be efficiently separated by carbon black granules with the separation method of residual Jiao, such that it is able to realize observing under a scanning electron microscope the pattern of carbon black granules and residual Jiao.
In a kind of burned-coal fly ash, carbon black granules and the method for quantitatively determining of residual Jiao, comprise the steps:
In burned-coal fly ash described in any of the above-described embodiment, carbon black granules separates with the separation method of residual Jiao and obtains described floating and described precipitated phase;
Being respectively added in combustion boat by described floating with described precipitated phase, wherein, the clean quality of the described combustion boat for containing described floating phase is designated as m10, the clean quality of the described combustion boat for containing described precipitated phase is designated as m20;
Float mutually and described precipitated phase is dried process to remove described liquid dispersant to described respectively, the described carbon black granules obtained and described combustion boat weigh after quality be designated as m11, described residual burnt and described combustion boat weigh after quality be designated as m21;
The described carbon black granules obtained after dried and described residual Jiao are carried out complete burn processing respectively, described carbon black granules weigh with described combustion boat after burning completely after quality be designated as m12, described residual Jiao weigh with described combustion boat after burning completely after quality be designated as m22, carbon black granules is carried out quantitative analysis with residual Jiao;
The quality of described carbon black granules is m11-m12, described carbon black granules weight/mass percentage composition in described burned-coal fly ash is (m11-m12)/(m11-m10+m21-m20) * 100%; The quality of described residual Jiao is m21-m22, described residual Jiao weight/mass percentage composition in described burned-coal fly ash is (m21-m22)/(m11-m10+m21-m20) * 100%.
Wherein in an embodiment, described method for quantitatively determining calculates the step of meansigma methods after also including the weight/mass percentage composition of described carbon black granules and described residual Jiao repeatedly measuring in described burned-coal fly ash.
Wherein in an embodiment, described is repeatedly at least 3 times.
Wherein in an embodiment, described liquid dispersant is ethanol, and the temperature of described dried is more than 78.4 DEG C.
Wherein in an embodiment, it is put into the described combustion boat containing described carbon black granules with the described combustion boat containing described residual Jiao to carry out burn processing in Muffle furnace that the described described carbon black granules to obtaining after dried and described residual Jiao carry out complete burn processing respectively, and the temperature of described Muffle furnace is 800��830 DEG C.
In this burned-coal fly ash, the method for quantitatively determining of carbon black granules and residual Jiao is of poor quality by what measure before and after burning, it is possible to carbon black granules in simultaneous quantitative burned-coal fly ash and the content of residual Jiao, and then can the quality of effective evaluation burning of coal effect and burned-coal fly ash.
In a word, in the burned-coal fly ash of the present invention carbon black granules and residual Jiao separate and equipment, articles for use needed for method for quantitatively determining, instrument is fairly simple is easy to get, low price, is highly suitable for the practical operation of power plant. Compared to instruments such as traditional thermogravimetric analyzer and Andersen particles hit device, elemental analyser, above-mentioned separation and method for quantitatively determining greatly reduce use cost, and simplify operating process, such that it is able to improve the efficiency separated with quantitative assay.
Detailed description of the invention
For the ease of understanding the present invention, below with reference to relevant drawings and specific embodiment, the present invention is described more fully. Accompanying drawing gives presently preferred embodiments of the present invention. But, the present invention can realize in many different forms, however it is not limited to embodiment described herein. On the contrary, the purpose providing these embodiments is to make the understanding to the disclosure more thorough comprehensively.
As it is shown in figure 1, the separation method of carbon black granules and residual Jiao in the burned-coal fly ash of an embodiment, comprise the steps:
Step S110: use liquid dispersant to disperse burned-coal fly ash, and carry out ultrasonic vibration, obtain burned-coal fly ash suspension.
This burned-coal fly ash can directly be taken from the ash buckets such as boiler fired coal, coal-fired due to imperfect combustion, can contain the unburned carbon such as carbon black granules and residual Jiao in flying dust.
The liquid dispersant of present embodiment selects ethanol. It is understood that in other embodiments, this liquid dispersant can also select the liquid flux such as water, ethanol water.
The power of the ultrasonic vibration of present embodiment selects 0.4kW. It is understood that in other embodiments, it is any power between 0.1��0.5kW that the power of ultrasonic vibration can also be selected.
Step S120: stand burned-coal fly ash suspension and make residual Jiao precipitate, thus layering occur in liquid dispersant in carbon black granules and residual Jiao, generates the precipitated phase mutually and containing residual Jiao that floats containing carbon black granules.
Step S130: collect respectively and float mutually and precipitated phase, namely realizes separating carbon black granules in burned-coal fly ash and residual Jiao.
Density variation due to carbon black granules Yu residual Jiao, after the liquid dispersant contained in burned-coal fly ash after being disperseed by ultrasonic vibration stands a period of time, carbon black granules and residual Jiao can be layered, thus generating the precipitated phase mutually with containing residual Jiao that floats containing carbon black granules. Collect this floating phase and precipitated phase respectively, and carbon black granules and residual Jiao can be obtained after dry removing liquid dispersant.
Further, in the present embodiment, this separation method also includes repeating the step separating and purifying carbon black granules and residual Jiao respectively. This repeated isolation respectively purification carbon black granules specifically include with the step of residual Jiao: continue adding liquid dispersant in the precipitated phase collected, and the floating respectively liquid dispersant containing precipitated phase and back collected is sequentially carried out ultrasonic vibration mutually and standing processes, then collect respectively stand after the floating phase of layering and precipitated phase. In the present embodiment, above-mentioned steps S110-step S130 is repeated once. It is understood that in other embodiments, separation can be repeated and till purification carbon black granules does not have precipitated phase to occur until floating with residual Jiao after ultrasonic vibration and standing process respectively.
In this burned-coal fly ash, carbon black granules in burned-coal fly ash and residual Jiao can be efficiently separated by carbon black granules with the separation method of residual Jiao, such that it is able to realize observing under a scanning electron microscope the pattern of carbon black granules and residual Jiao.
Additionally, present embodiment additionally provides the method for quantitatively determining of carbon black granules and residual Jiao in a kind of burned-coal fly ash, as in figure 2 it is shown, this method for quantitatively determining comprises the steps:
Step S210: separate with the separation method of residual Jiao according to carbon black granules in above-mentioned burned-coal fly ash and obtain floating mutually and precipitated phase.
Separate including the separation method used described in above-mentioned present embodiment or other embodiments and obtain floating mutually and precipitated phase.
Step S220: be respectively added in combustion boat by floating and precipitated phase, wherein, the clean quality of the combustion boat for containing floating phase is designated as m10, the clean quality of the combustion boat for containing precipitated phase is designated as m20��
First combustion boat adds float with precipitated phase before, also include the step that combustion boat is weighed, respectively obtain and float mutually and the clean quality of the combustion boat of precipitated phase for containing.
Combustion boat used by present embodiment is crucible. It is understood that in other embodiments, combustion boat can also be other potteries or the vessel etc. being available for inclusions burning of metal making.
Step S230: respectively to floating mutually and precipitated phase is dried process to remove liquid dispersant, the carbon black granules obtained and combustion boat weigh after quality be designated as m11, residual Jiao and combustion boat weigh after quality be designated as m21��
Dried mode described in present embodiment is will to contain the phase combustion boat with precipitated phase that floats as in air dry oven respectively, it is dried process to evaporate this liquid dispersant of removing at higher than temperature more than liquid dispersant boiling point, as when liquid dispersant is ethanol, dry temperature can be any temperature etc. ethyl alcohol boiling point more than 78.4 DEG C such as 120 DEG C of grades.
Step S240: the carbon black granules obtained after dried and residual Jiao are carried out complete burn processing respectively, carbon black granules weigh with combustion boat after burning completely after quality be designated as m12, residual Jiao weigh with combustion boat after burning completely after quality be designated as m22, carbon black granules is carried out quantitative analysis with residual Jiao.
The quality of carbon black granules is m11-m12, carbon black granules weight/mass percentage composition in burned-coal fly ash is (m11-m12)/(m11-m10+m21-m20) * 100%; The quality of residual Jiao is m21-m22, residual Jiao weight/mass percentage composition in burned-coal fly ash is (m21-m22)/(m11-m10+m21-m20) * 100%.
Complete burn processing described in present embodiment is the combustion boat containing carbon black granules and combustion boat containing residual Jiao to put into a period of time in Muffle furnace carry out complete burn processing, as for different sample sizes, can set that the temperature of Muffle furnace is 800��830 DEG C, such as 815 DEG C etc., standing time was such as 30 minutes etc.
Further, in the present embodiment, for ensureing the reliability of experimental result, the step of meansigma methods after the carbon black granules that this method for quantitatively determining also includes repeatedly measuring in burned-coal fly ash and the weight/mass percentage composition of residual Jiao, is calculated, as inferior in repeated at least 3.
In above-mentioned burned-coal fly ash, the method for quantitatively determining of carbon black granules and residual Jiao is of poor quality by what measure before and after burning, it is possible to carbon black granules in simultaneous quantitative burned-coal fly ash and the content of residual Jiao, and then can the quality of effective evaluation burning of coal effect and burned-coal fly ash.
In this burned-coal fly ash carbon black granules and residual Jiao separate and equipment, articles for use needed for method for quantitatively determining, instrument is fairly simple is easy to get, low price, is highly suitable for the practical operation of power plant. Compared to instruments such as traditional thermogravimetric analyzer and Andersen particles hit device, elemental analyser, above-mentioned separation and method for quantitatively determining greatly reduce use cost, and simplify operating process, such that it is able to improve the efficiency separated with quantitative assay, it is possible to wide popularization and application is in the test analysis field of coal-burning power plant.
It it is below specific embodiment part
One, material, equipment:
Burned-coal fly ash sample some (source: green hill, Wuhan steam power plant), ethanol, test tube are some, two, crucible, ultrasonic washing instrument (model and manufacturer: KX-1012, imperial or royal seal ultrasonic washing unit (Beijing) company limited of section), air dry oven, Muffle furnace, electronic balance (precision 0.1mg);
Take two test tubes label test tube 1 and test tube 2 respectively, two crucibles label crucible 1 and crucibles 2 respectively.
Two, separation and quantitative assay:
(1). weigh 0.01��0.02g burned-coal fly ash sample, join in test tube 1.
(2). adding 20ml ethanol in test tube 1, and put into by test tube 1 with 0.4kW power shock 5 minutes in ultrasonic washing instrument, the burned-coal fly ash in test tube 1 and ethanol are dispersed into suspension.
(3). take out test tube 1, and stand 60 minutes, suspension separates into two parts, it is designated as floating phase (the 18-19ml suspension on upper strata) and precipitated phase (the 1-2ml mixture of lower floor) respectively, owing to the density of carbon black granules is less than residual Jiao, carbon black granules is split into and floats in mutually, and residual Jiao is then split in precipitated phase.
(4). by floating phase transfer to test tube 2, test tube 1 continuously adds 20ml ethanol.
(5). test tube 1, test tube 2 are repeated the operation 1 time of step (2), (3).
(6). weigh the quality of crucible 1 and crucible 2, be designated as m respectively10And m20��
(7). test tube 1 is concentrated mutually with the floating in test tube 2 and transfers in crucible 1, the precipitated phase in test tube 1 and test tube 2 is concentrated and transfers in crucible 2.
(8). will be equipped with the crucible 2 of the crucible 1 of floating phase and precipitated phase and put in air dry oven, baking temperature 120 DEG C is set, after ethanol evaporates completely, take out crucible 1 and crucible 2.
(9). again weigh the quality of crucible 1 and crucible 2, be designated as m respectively11And m21��
(10). crucible 1 and crucible 2 are put in Muffle furnace, sets muffle furnace 815 DEG C, place 30 minutes, so that the carbon black granules in crucible 1 and residual Jiao in crucible 2 are fully burnt.
(11). weigh the quality of the crucible 1 after burning and crucible 2, be designated as m12And m22��
The quality being derived from carbon black granules is m11-m12, carbon black granules percentage composition in burned-coal fly ash is (m11-m12)/(m11-m10+m21-m20) * 100%; The quality of residual Jiao is m21-m22, residual Jiao percentage composition in burned-coal fly ash is (m21-m22)/(m11-m10+m21-m20)*100%��
For ensureing the reliability of experimental result, every kind of burned-coal fly ash sample needs to repeat at least 3 times, and final result is averaged, and result is table 1 below such as:
Table 1
Note: above mass unit: g.
Embodiment described above only have expressed the several embodiments of the present invention, and it describes comparatively concrete and detailed, but therefore can not be interpreted as the restriction to the scope of the claims of the present invention. It should be pointed out that, for the person of ordinary skill of the art, without departing from the inventive concept of the premise, it is also possible to making some deformation and improvement, these broadly fall into protection scope of the present invention. Therefore, the protection domain of patent of the present invention should be as the criterion with claims.