CN110918063B - Preparation process of environment-friendly adsorption material and adsorption testing system - Google Patents
Preparation process of environment-friendly adsorption material and adsorption testing system Download PDFInfo
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Abstract
The active carbon adsorption system consists of a plurality of components such as a test cavity, a pipeline and a loading device for adsorption particles, the active carbon in the active carbon adsorption system can monitor the concentration change of pollutants before and after adsorption of the active carbon, can provide accurate reference for determining the service life of the active carbon, can judge whether the active carbon needs to be replaced, and has the advantages of simple structure and accurate detection.
Description
Technical Field
The invention relates to the field of environmental protection, in particular to an activated carbon preparation process, an adsorption test system and an adsorption test method.
Background
The active carbon is a carbon source substance, is an excellent environment-friendly adsorption material, has a product with a large number of pore structures after carbonization and physical activation or chemical activation treatment, has no energy consumption, no toxicity, high specific surface area and good adsorption capacity, and is an adsorbent material widely applied to pollutant removal at present, such as purification of drinking water, industrial wastewater and domestic sewage, purification of factory waste gas and toxic gas and the like.
The application of activated carbon in gas phase is mainly embodied in the aspects of waste gas treatment, separation and purification of industrial gas, recovery of volatile organic solvent and the like. The activated carbon can be used for treating waste gas containing sulfur dioxide, nitrogen oxide, hydrogen sulfide, carbon monoxide, arsenic, mercury, carbon nitride, dioxin and the like, and plays a vital role in environmental protection aspects such as air pollution treatment and the like.
Although the activated carbon has good adsorption capacity, the activated carbon still has adsorption 'life', the absorption of the activated carbon reaches a saturation state, and the activated carbon cannot absorb more polluted gas, and can even become a second pollution source, but at present, no convenient and practical monitoring means exists, so that many users can only determine the service life of the activated carbon filter according to a specified period or by experience, and great errors and even problems are caused, and therefore, a simple, convenient and accurate-operation testing device system is urgently needed to solve the problems.
Disclosure of Invention
Accordingly, in view of the disadvantages in the related art, examples of the present invention are provided to substantially solve one or more problems due to limitations and disadvantages of the related art, to substantially improve safety and reliability, and to effectively protect equipment.
According to the technical scheme provided by the invention, the test system can test the adsorption capacity of adsorption particles and comprises a test cavity, the test cavity is connected with a gas generation device through a communication pipeline, a switch valve and a flow control device are arranged on the communication pipeline, a temperature control device and a humidity control device are further communicated with one side of the test cavity, a loading device is arranged in the test cavity and used for loading the adsorption particles, the adsorption particles in the loading device are loaded and compacted by pressure, the loading device is arranged at the rear part of a pipeline joint, the front part of the pipeline joint extends out of the test cavity, the head part of the pipeline joint is communicated with a first branch of a three-way pipeline, a second branch of the three-way pipeline is connected with a flame ionization detection device, the flame ionization detection device is connected with a recorder, and the recorder can be used for drawing a curve graph from the time of adsorption particles from the beginning of gas adsorption to the time of the absorption and the time of the The second branch is also connected with a needle valve and a diaphragm pump, and the third branch of the three-way pipeline is connected with a filtering device/a washing device.
Further, loading attachment is the toper including loading the body, and the edge of loading the body is equipped with the supporting part, and the supporting part supplies pressure to load and supports, loads this internal chassis that is equipped with, is equipped with a plurality of through-hole on the chassis, and the place ahead on chassis is equipped with the lid dish, also is equipped with a plurality of through-hole on the lid dish, and the adsorbed particle is located between chassis and the lid dish, and the size of adsorbed particle is greater than the size of chassis, lid dish through-hole.
Furthermore, the pressure device comprises a beam main body, two ends of the beam main body are respectively provided with a pillar, the two pillars are matched with the supporting grooves of the supporting parts, the middle part of the beam main body is provided with a driving screw, one end of the driving screw is provided with a pressing plate, the other end of the driving screw is provided with an inner hexagon nut, and a torque wrench is matched with the inner hexagon nut to apply pressure.
Furthermore, the surface of the active carbon is impregnated with copper ions, silver ions, molybdenum ions or magnesium ions.
The invention provides a preparation process of activated carbon, and simultaneously provides an activated carbon adsorption test system and an adsorption test method.
Drawings
FIG. 1 is a schematic diagram of an adsorption test system of the present invention.
Fig. 2 is a schematic view of the loading device and the pressure device of the present invention.
FIG. 3 is a schematic view of the adsorption process of the present invention.
FIG. 4 is a schematic diagram of a recording curve according to the present invention.
Detailed Description
The present invention will be further described with reference to the following specific examples.
The present invention will be described in detail below with reference to specific embodiments shown in the drawings. These embodiments are not intended to limit the present invention, and structural, methodological, or functional changes made by those skilled in the art according to these embodiments are included in the scope of the present invention. The application of the principles of the present invention will be further described with reference to the accompanying drawings and specific embodiments.
The environment-friendly adsorption material related by the invention is activated carbon, the activated carbon consists of more than nine carbon and trace amounts of sulfur, hydrogen, oxygen and nitrogen, the appearance is generally black granular or powdery, if the activated carbon is in an irregular structure viewed by SEM, the activated carbon contains a large number of holes, and the holes can be divided into the following parts according to the size: macropores, mesopores, and micropores, the surface characteristics of activated carbon are represented by the pore distribution, wherein the greater the amount of micropores, the higher the surface area of activated carbon, and theoretically, the better the adsorption performance.
The invention utilizes a hydrothermal synthesis method to carbonize glucose into a carbon sphere structure, the carbon sphere has the characteristics of high stability, physical and chemical properties, adjustable specific surface area and the like, is very suitable for being used as a precursor of active carbon, and is doped with K with different proportions2CO3Chemical activation is carried out to prepare the active carbon with more mesopore structures.
The active carbon is prepared by the following process:
A. adding 30g of glucose into 100mL of deionized water, and stirring on a magnetic stirrer until the glucose is completely dissolved;
B. pouring the mixed solution into a polytetrafluoroethylene container, placing the container into a high-pressure tank, and placing the container into a high-temperature furnace for reaction, wherein the reaction temperature is set to be 190 ℃ and the time is 24 hours;
C. after the reaction is finished, filtering by using a vacuum pump and repeatedly washing by using deionized water until the filtrate is clear and colorless,
D. putting the obtained product in a drying oven at 105 ℃ for drying for 24 hours to obtain carbon spheres;
E. will K2CO3The powder was dissolved in 100mL deionized water to form K2CO3Solution, placing the obtained carbon spheres in K2CO3In solution, wherein the carbon spheres are reacted with K2CO3The mass ratio of the powder is 1:3, and the mixed solution is placed in a 65 ℃ oven to be dried for 24 hours;
F. putting the product obtained in the step E into a magnetic crucible container, putting the container into a high-temperature furnace for reaction, setting the reaction temperature to be 800 ℃, and keeping the reaction time to be 4 hours;
G. repeatedly flushing and washing with 0.1M HC1 and deionized water until the filtrate is clear and colorless;
H. and D, placing the product obtained in the step G in an oven at 105 ℃ for drying for 24 hours to obtain the activated carbon.
It is specifically stated that K is avoided2CO3The solution is mixed with carbon spheres to generate water vapor at high temperature, so that the step E is specially adopted to mix K2CO3The mixture of the solution and the carbon spheres is dried at 65 ℃ and then activated, the yield can reach 3-3.6 g, the yield is 11.72-11.98%, and the yield of the activated carbon is remarkably improved.
The active carbon can also be impregnated with copper ions, silver ions, molybdenum ions or magnesium ions, wherein Cu is +2 valent, Ag is +1 valent, Mo is +6 valent, and Zn is +2 valent, specifically, the impregnated active carbon is impregnated by four chemicals of copper carbonate, silver nitrate, ammonium molybdate, zinc carbonate and the like, and the four transition metal ions play a role in the impregnated active carbon in catalysis of chemical adsorption and detoxification.
The active carbon is a material with high porosity, which can absorb toxic gas on the surface of the pores by van der Waals force generated between the pore structure and the molecules, and the specific surface area of the active carbon reaches 1000 m2And the gas molecules are contacted and collided with the activated carbon when passing through the activated carbon layer, and when the gas molecules are collided with the surface of the activated carbon, the toxic gas is absorbed and then trapped on the surface of the adsorption substance to be filtered.
The maximum quantity that unit activated carbon can adsorb is called "adsorption capacity", different materials or different gases are adsorbed, and the adsorption capacity is different. The residence time of the exhaust gas in the activated carbon adsorption unit until the gas flow passes through the activated carbon layer is called "residence time", and in general, the longer the residence time, the more sufficient the adsorption.
At present, the harm and the variety of various chemical harmful gas agents are various, however, the molecular weight of general chemical harmful gas is far larger than the molecular weight of air, when facing chemical waste gas with small molecular weight, whether the active carbon can effectively adsorb and intercept the chemical harmful gas with the molecular weight smaller than the molecular weight of air is very important, for example, when hydrogen cyanide is used, compared with the molecular weight of air about 28.8, the density of air vapor is about 1, compared with the hydrogen cyanide toxic gas is similar to air, if the hydrogen cyanide toxic gas can successfully adsorb and intercept harmful gas hydrogen cyanide with small molecular weight, under the same adsorption test condition, the adsorption life capability, namely the saturation penetration time, of the chemical harmful gas with large molecular weight is longer, therefore, the chemical harmful gas hydrogen cyanide with the property similar to air is used as the adsorption penetration gas for test.
The specific gas to be adsorbed by the device is hydrogen cyanide, the temperature is 22 +/-2 ℃, the humidity is 55 +/-5% RH, the gas concentration is 4.0 mg/L, the flow is 30L/min, the penetration concentration is 1 ppm, the concentration of the gas hydrogen cyanide penetrating out of the active carbon is sensed by using a flame ionization detection device, a graph from the time of adsorbing harmful gas to the time of penetrating out after adsorption saturation is drawn by a recorder, and finally the saturation penetration time of a straight line part (namely the time of a T0-T1 straight line segment) on the penetration graph is calculated.
Specifically, as shown in fig. 1, the testing system of the present application includes a testing chamber, the testing chamber is connected to a gas generating device through a communication pipeline, a switch valve and a flow control device are disposed on the communication pipeline, a temperature control device and a humidity control device are further communicated to one side of the testing chamber, a loading device is disposed in the testing chamber, the loading device is used for loading adsorption particles, the adsorption particles in the loading device are loaded and compacted by pressure, the loading device is mounted at the rear part of a pipeline joint, the front part of the pipeline joint extends out of the testing chamber, the head part of the pipeline joint is communicated with a first branch of a three-way pipeline, a second branch of the three-way pipeline is connected to a flame ionization detection device, the flame ionization detection device is connected to a recorder, the recorder can be used for plotting a graph from the time of adsorption particles from the beginning of gas, the second branch is also connected with a needle valve and a diaphragm pump, and the third branch of the three-way pipeline is connected with a filtering device/a washing device.
It should explain very much, loading attachment is including loading body and connecting tube portion, wherein, it is the toper to load the body, the edge of loading the body is equipped with the supporting part, the supporting part supplies pressure device to support, load this internal chassis that is equipped with, be equipped with a plurality of through-hole on the chassis, the place ahead on chassis is equipped with the cover plate, also be equipped with a plurality of through-hole on the cover plate, adsorption particles is located between chassis and the cover plate, adsorption particles's size is greater than the chassis, the size of cover plate through-hole, the chassis is the same with the size of cover plate and be dismantled and assembled setting on loading the body, connecting tube portion integrated into one piece is in the front portion of loading the body, connecting tube portion is cylindrical, connecting tube portion joint or screwed connection are in.
The external connection who loads the body has the test copper line, and the inside of loading the body has also installed the test copper line, and two sections test copper lines are connected with the multimeter, and the multimeter can be used for measuring the resistance value before the specific gaseous hydrogen cyanide of active carbon adsorption wears out to the resistance value of measuring active carbon once more after the saturation wears out, can know the change of the resistance value around the active carbon adsorption hydrogen cyanide gas body.
Pressure device includes the crossbeam main part, and the both ends of crossbeam main part are equipped with a pillar respectively, and two pillars cooperate with the support groove of support portion, and the pillar can be the screw rod, can conveniently adjust the height of crossbeam main part like this, facilitates the use, and the middle part of crossbeam main part is equipped with drive screw, and drive screw's one end is equipped with the clamp plate, and drive screw's the other end is equipped with hexagon nut in, exerts pressure by torque wrench cooperation hexagon nut in.
The active carbon adsorption test method comprises the following steps:
1) turning on a power supply of the gas generating device; so that the gas generating device starts to work;
2) placing the base plate in the loading body, flatly filling and filling the activated carbon particles in the loading body, packaging the upper cover plate, connecting the pressing plate to the bottom end of the driving screw rod, matching the two supports with the corresponding supporting grooves to enable the beam main body to be positioned right above the loading body, operating the hexagon socket head cap nut by using a torque wrench, driving the pressing plate to apply pressure downwards by using the driving bolt to compact the activated carbon particles, and then taking the pressure device off the loading body; it should be noted that, for the diameter of the base plate and the cover plate of this embodiment is 104mm, the weight of the activated carbon filled in the loading body is about 63g, and the carbon bed thickness is 16mm, the torsion is uniformly set to 8Kgf-cm by using a torsion wrench, and the carbon bed thickness is 14mm after being compacted, so as to properly compact (densify) the activated carbon, avoid loosening or causing uneven height (thickness) of the carbon bed in the loading body, and simultaneously not cause the activated carbon to break (crack), and have proper expiratory impedance, so as to avoid the change of a flow field caused by the flow of the test gas flowing through the inside of the loading body to generate turbulence, and influence the test adsorption saturation wear-out time;
3) opening the door of the test cavity, putting the compacted active carbon into the loading device, and closing the door of the test cavity;
4) opening a switch valve on the communication pipeline, and adjusting the flow control device to be 30L/min;
5) operating the temperature control device and the humidity control device such that the temperature is 22 + -2 deg.C and the humidity is 55 + -5% RH;
6) starting the flame ionization detection device and the recorder;
7) igniting the flame ionization detection device, starting the recorder to operate, and recording the time of the starting point of the straight line as T0;
8) starting the diaphragm pump and setting the flow rate to be 1L/min;
9) when the activated carbon adsorbs the test gas to be saturated, the test gas penetrates out of the activated carbon, the flame ionization detection device detects the test gas, the drawing base line of the recorder deviates, as shown in fig. 4, the recording straight line becomes a recording arc line, and the time from the recording straight line to the recording arc line is T1; further, the flame ionization detection device of the invention detects the concentration of the gas exhausted from the activated carbon in the loading body in the whole process, and transmits a signal to the recorder, when the activated carbon is not saturated and exhausted, the flame ionization detection device can not detect hydrogen cyanide gas, the recorder draws a straight line segment, and a drawing base line draws an arc curve along with the increase of the concentration of the hydrogen cyanide gas in the process of the exhaust of the activated carbon along with the adsorption of the gas, namely an exhaust curve chart;
10) calculating the saturation penetration time of the test gas by the following formula: the saturation exit time = T1-T0, and the saturation exit time can be obtained by the following formula: t = L × 60/V, where T is the saturation exit time, L is the length of the recording line, and V is the print rate of the recorder; for example, the printing speed of the recorder of the embodiment is 100mm/h, so the time of every 1 mm of the recorder is 0.6 min, if the recording straight line is 40mm, the saturation penetration time (min) =40(mm) × 60(min)/100(mm) =24 (min);
11) closing each pipeline valve, and taking out the loading device when the cavity to be tested has no test gas.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (3)
1. An active carbon adsorption test method is completed by a test system which comprises a test cavity connected with a gas generating device through a communication pipeline, a switch valve and a flow control device are arranged on the communication pipeline, a temperature control device and a humidity control device are further communicated on one side of the test cavity, a loading device is arranged in the test cavity and used for loading the active carbon, the active carbon positioned in the loading device is compacted by a pressure device, the loading device is arranged at the rear part of a pipeline joint, the front part of the pipeline joint extends out of the test cavity, the head part of the pipeline joint is communicated with a first branch of a three-way pipeline, a second branch of the three-way pipeline is connected with a flame ionization detection device, the flame ionization detection device is connected with a recorder, the recorder can be used for drawing a curve chart from the time of starting to adsorb gas to the time of penetrating out of adsorption saturation of the activated carbon, the second branch is also connected with a needle valve and a diaphragm pump, and the third branch of the three-way pipeline is connected with a filtering device/a washing device; the loading device comprises a loading body, the loading body is conical, a supporting part is arranged at the edge of the loading body and is used for supporting the pressure device, a base plate is arranged in the loading body, a plurality of through holes are formed in the base plate, a cover disc is arranged in front of the base plate, a plurality of through holes are also formed in the cover disc, the active carbon is positioned between the base plate and the cover disc, and the size of the active carbon is larger than that of the through holes of the base plate and the cover disc; the pressure device comprises a beam main body, two ends of the beam main body are respectively provided with a pillar, the two pillars are matched with the supporting grooves of the supporting parts, the middle part of the beam main body is provided with a driving screw rod, one end of the driving screw rod is provided with a pressure plate, the other end of the driving screw rod is provided with an inner hexagon nut, and a torque wrench is matched with the inner hexagon nut to apply pressure; the method is characterized by comprising the following steps:
1) turning on a power supply of the gas generating device; so that the gas generating device starts to work;
2) placing the base plate in the loading body, flatly filling and filling the activated carbon particles in the loading body, packaging the upper cover plate, connecting the pressing plate to the bottom end of the driving screw rod, matching the two supports with the corresponding supporting grooves to enable the beam main body to be positioned right above the loading body, operating the hexagon socket head cap nut by using a torque wrench, driving the pressing plate to apply pressure downwards by using the driving bolt to compact the activated carbon particles, and then taking the pressure device off the loading body;
3) opening the door of the test cavity, putting the compacted active carbon into the loading device, and closing the door of the test cavity;
4) opening a switch valve on the communication pipeline, and adjusting the flow control device to be 30L/min;
5) operating the temperature control device and the humidity control device so that the temperature is 22 + -2 ℃ and the humidity is 55 + -5% RH;
6) starting the flame ionization detection device and the recorder;
7) igniting the flame ionization detection device, starting the recorder to operate, and recording the time of the starting point of the straight line as T0;
8) starting the diaphragm pump and setting the flow rate to be 1L/min;
9) when the activated carbon adsorbs test gas to be saturated, the test gas penetrates out of the activated carbon, the flame ionization detection device detects the test gas, the drawing base line of the recorder deviates, the recording straight line becomes a recording arc line, and the time from the recording straight line to the recording arc line is T1;
10) calculating the saturation penetration time of the test gas by the following formula: saturation exit time = T1-T0;
11) closing each pipeline valve, and taking out the loading device when the cavity to be tested has no test gas.
2. The activated carbon adsorption test method of claim 1, wherein the activated carbon is prepared by the following process:
A. adding 30g of glucose into 100mL of deionized water, and stirring on a magnetic stirrer until the glucose is completely dissolved;
B. pouring the mixed solution obtained in the step A into a polytetrafluoroethylene container, placing the container into a high-pressure tank, and placing the container into a high-temperature furnace for reaction, wherein the reaction temperature is set to 190 ℃ and the reaction time is 24 hours;
C. after the reaction is finished, filtering by using a vacuum pump and repeatedly washing by using deionized water until the filtrate is clear and colorless,
D. putting the obtained product in a drying oven at 105 ℃ for drying for 24 hours to obtain carbon spheres;
E. will K2CO3The powder was dissolved in 100mL deionized water to form K2CO3Solution, placing the obtained carbon spheres in K2CO3In solution, wherein the carbon spheres are reacted with K2CO3The mass ratio of the powder is 1:3, and the mixture is mixedPutting the solution into a 65 ℃ oven to be dried for 24 hours;
F. putting the product obtained in the step E into a magnetic crucible container, putting the container into a high-temperature furnace for reaction, and setting the reaction temperature to be 800 ℃ for 4 hours;
G. repeatedly flushing and washing with 0.1M HC1 and deionized water until the filtrate is clear and colorless;
H. and D, placing the product obtained in the step G in an oven at 105 ℃ for drying for 24 hours to obtain the activated carbon.
3. The activated carbon adsorption test method of claim 1, wherein the surface of the activated carbon is further impregnated with copper ions, silver ions, molybdenum ions or magnesium ions.
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