CN109060591A - A kind of evaluating apparatus and evaluation method for escaping gas performance of the adsorbent - Google Patents
A kind of evaluating apparatus and evaluation method for escaping gas performance of the adsorbent Download PDFInfo
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- CN109060591A CN109060591A CN201810762527.6A CN201810762527A CN109060591A CN 109060591 A CN109060591 A CN 109060591A CN 201810762527 A CN201810762527 A CN 201810762527A CN 109060591 A CN109060591 A CN 109060591A
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Abstract
The invention discloses a kind of evaluating apparatus and evaluation method for escaping gas performance of the adsorbent, device includes gas absorption/desorption system and on-line analysis display system, gas absorption/desorption system includes first with gas cylinder, gas is divided into two branches through the first triple valve with gas cylinder by first, branch 1 is connect by the first gating component with VOC saturation generator, branch 2 is connect by the second gating component with water saturation generator, after VOC saturation generator and water saturation generator exports pipeline are converged by the second triple valve, it is connect respectively with reactor and on-line analysis display system through the 4th triple valve and the 5th triple valve, reactor outlet is connect through the 5th triple valve with on-line analysis display system, again by piping connection to tail gas absorption bottle.This evaluating apparatus and evaluation method, it is easy to operate, influence of the conditions such as gas composition, temperature, flow in adsorption process to adsorption capacity, and the reaction mechanism mechanism of reaction, the reactivation etc. of research adsorbent can be measured simultaneously.
Description
Technical field
The present invention relates to a kind of performance of the adsorbent evaluating apparatus and evaluation methods, and in particular to one kind is used for escaping gas
The evaluating apparatus and evaluation method of performance of the adsorbent
Background technique
With the swift and violent emergence of Industrial-Enterprises in China, various environmental problems come one after another, wherein volatile organic matter
(VOCs) pollution is gradually paid close attention to.Volatile organic matter (VOCs) refer under room temperature saturated vapor pressure be greater than 133.32Pa,
The gas chromatographies such as the organic compound of boiling point at 50~260 DEG C, including hydrocarbon, aldehyde, ketone, alcohol, ether, ester under normal pressure.In atmosphere
VOCs has the characteristics that many kinds of, from a wealth of sources, toxicity is big, concentration is relatively low but the total amount of pollutant is big, main source
Have: 1) stationary source, the exhaust gas of the industries such as petrochemical industry, pharmacy, coating material production discharge；2) moving source, the vehicles such as automobile row
The tail gas put；3) oil smoke of family's discharge.Although the VOCs proportion of anthropogenic discharge is less in atmosphere, most of VOCs tools
It is toxic, not only easily cause room air pollution, can also be acted in illumination and issue third contact of a total solar or lunar eclipse chemical reaction, cause depletion of the ozone layer,
The concentration of photochemical fog, secondary organic aerosol and atmosphere organic acid increases, and threatens to human health and atmospheric environment.
Adsorbent VOCs separation and in terms of be widely used, the adsorbent of Development of Novel is numerous sections
The direction that scholar makes great efforts, meanwhile, the screening of high activity adsorbent is also a difficult task, needs long time just can be with
It completes.Existing adsorbent evaluation device is suitable for that influence factor is less, and single factor test, the experiment of the Long-Term Simulations of multicycle work as research
When influence factor is more, need to take considerable time.
Summary of the invention
The purpose of the invention is to overcome the deficiencies of the prior art and provide a kind of waving for achievable many condition absorption test
The evaluating apparatus and evaluation method of hair property adsorbent performance.
Technical scheme is as follows:
A kind of evaluating apparatus for escaping gas performance of the adsorbent, including gas absorption/desorption system and online point
Display system is analysed,
Gas absorption/the desorption system includes first with gas cylinder, and first, which matches gas cylinder, is divided into gas through the first triple valve
Two branches, branch 1 are connect by the first gating component with VOC saturation generator, and branch 2 passes through the second gating component and water saturation
After generator connection, VOC saturation generator and water saturation generator exports pipeline are converged by the second triple valve, through the 4th threeway
Valve and the 5th triple valve are connect with reactor and on-line analysis display system respectively, and reactor outlet is through the 5th triple valve and online
Analysis shows that system connects, then by piping connection to tail gas absorption bottle；
The on-line analysis display system includes gas chromatographicanalyzer and computer, and the two is connected by Serial Port Line, gas phase
Chromatograph is connect with reactor outlet.
Gas absorption/the desorption system further includes second with gas cylinder, and second, which matches gas cylinder, passes through third triple valve and branch 1
Converge with 2 gas of branch.
First gating component and the second gating component are the two sets of ball valves being set side by side, wherein one group of ball valve is two
A concatenated ball valve connects VOC saturation generator (2) between two ball valves or water saturation generator (3), another group of ball valve is
One ball valve, both ends are connect with the inlet and outlet of VOC saturation generator (2) or water saturation generator (3) respectively, and gas passes through
After gating component, selectivity enters VOC saturation generator (2) or water saturation generator (3).The VOC saturation generator and
One constant temperature circulator is output and input pipeline and is connected, and deionized water is added in first constant temperature circulator or dehydrated alcohol is to follow
Ring liquid, bath temperature are -5 DEG C~95 DEG C；The water saturation generator is output and input pipeline phase with the second constant temperature circulator
Even, it is circulation fluid that deionized water is added in second constant temperature circulator, and bath temperature is 0 DEG C~95 DEG C.
Quartz ampoule built in the reactor and open type electric heating reacting furnace, upper end connection are located at the pressure outside reactor
Table, lower end connection are located at electric thermo-couple temperature inductor and temperature control panel outside reactor.
Described first matches gas cylinder for nitrogen steel gas cylinder, and second matches the VOC calibrating gas steel that gas cylinder is nitrogen or certain concentration
Gas cylinder；Described first connects pressure reducing valve with cylinder outlet with gas cylinder and second.
The branch 1, branch 2 and second on gas cylinder pipeline, along gas flow direction be successively arranged ball valve, filter,
Mass flowmenter and check valve, the filter are connect with pressure gauge, and the flowmeter is connect with control instrument, for precisely controlling
Flow processed.
The present invention also provides a kind of evaluation methods of escaping gas performance of the adsorbent, include the following steps:
(1) adsorbent tabletting to be measured is sieved, the adsorbent of certain partial size is made, weighs a certain amount of adsorbent and is placed in instead
It answers in the quartz ampoule of device；
(2) first are set as nitrogen with gas cylinder, adjust the first triple valve, and gas is divided into all the way or two branches, is adjusted
First gating component, 1 gas-selectively of branch enter VOC saturation generator；Adjust the second gating component, the selection of 2 gas of branch
Property enters water saturation generator；The second triple valve is adjusted, branch 1 and 2 gas of branch are converged；
(3) the second VOC Standard Gases for being set as nitrogen or certain concentration with gas cylinder with bottle with gas cylinder or by second are closed
Body, wherein when being set as the VOC calibrating gas of nitrogen or certain concentration, adjust third triple valve, make itself and branch 1 and/or branch
2 gas of road converges；
(4) the 5th before the 4th triple valve and gas chromatograph after the gas of all branches converges, before adjusting reactor
Triple valve makes mixed gas selectively enter reactor reaction or be directly entered gas chromatograph and is analyzed, wherein gas into
It after entering reactor, with the adsorbent haptoreaction in reactor, is discharged from reactor lower end, into chromatographic, remains
Residual air body discharges after entering tail gas absorption bottle by the road from gas chromatograph gas outlet；
(5) it according to the data measured, obtains the working curve of surveyed adsorbent, judges absorption/Desorption Energy of adsorbent
Power.
VOC saturation generator is connected with the first constant temperature circulator through outputting and inputting pipeline in the step (2), and described
Add deionized water in one constant temperature circulator or dehydrated alcohol is circulation fluid, bath temperature is -5 DEG C~95 DEG C；Water saturation generator
It is connected with the second constant temperature circulator through outputting and inputting pipeline, in second constant temperature circulator plus deionized water is circulation fluid,
Bath temperature is 0 DEG C~95 DEG C；Reactor is by temperature programmed control in the step (4), for temperature of reactor to be arranged.
In the step (2) and step (3), branch 1, branch 2 and second on gas cylinder pipeline, along gas flow direction according to
Secondary to be equipped with ball valve, filter, mass flowmenter and check valve, the filter is connect with pressure gauge, described for measuring pressure
Mass flowmenter is connect with control instrument, for being precisely controlled flow.
It is measurement including breakthrough curve and adsorbance, de- the invention has the beneficial effects that the test of achievable kinds of experiments
The conditions pair such as gas composition, temperature, humidity, air speed, loadings, partial size are tested and probed into attached aptitude tests, sorbent life
The influence of adsorption capacity, meanwhile, this evaluating apparatus and evaluation method have easy to operate, perfect in shape and function, accuracy high, repeated
The advantages that good.
Usefulness of the present invention also resides in the flow that each branch can be accurately controlled by mass flowmenter, accuracy
It is high；It, can meanwhile in such a way that constant temperature circulator is combined with saturation generator and the mode of temperature regulating device and combination of reactors
One species are evaluated under different condition (reactant concentration is different, water vapour content is different and reaction temperature is different) to realize
Adsorbent, substantially increase the efficiency of research and development of adsorbent, shorten R&D process.
Detailed description of the invention
Fig. 1 is schematic structural diagram of the device of the invention.
Wherein, match gas cylinder at 1: the first；2:VOC saturation generator；3: water saturation generator；4: reactor；5: tail gas bottle；6:
Gas chromatograph；7: computer；: match gas cylinder at 8: the second；9: the first constant temperature circulators；10: the second constant temperature circulators；SV1: the first choosing
Logical component；SV2: the second gating component；TV1: the first triple valve；TV2: the second triple valve；TV3: third triple valve；TV4: the four
Triple valve；TV5: the five triple valve；BV: ball valve；F: filter；FM: mass flowmenter；CV: check valve
Specific embodiment
Invention is further described in detail with reference to the accompanying drawings and detailed description, but protection scope of the present invention
It is not limited to the content.
A kind of the embodiment of the present invention 1 are as follows: evaluating apparatus for escaping gas performance of the adsorbent
As shown in Figure 1, adsorbent evaluation device of the invention, including gas absorption/desorption system and on-line analysis are shown
System, wherein gas absorption/desorption system includes first with gas cylinder 1, and first, which matches gas cylinder 1, may be configured as nitrogen steel gas cylinder, through subtracting
It accesses in gas circuit after pressure valve decompression, is divided to by the first triple valve TV1 for two branches.
Its pressure value is measured by pressure gauge after ball valve BV, filter F in branch 1, subsequently into mass flow control
Device FM metering processed, flowmeter are connect with control instrument, can be precisely controlled flow, be then passed through check valve CV, adjust gating component
SV1 may be selected to enter or do not enter VOC saturation generator 2.
Above-mentioned VOC saturation generator 2 is connected with the first constant temperature circulator 9 through outputting and inputting pipeline, constant temperature circulator 9
Interior plus deionized water or dehydrated alcohol are circulation fluid, and -5 DEG C of bath temperature~95 DEG C are adjustable.The N of certain flow2Flow through saturation hair
VOC solution in raw device, carries out certain density VOC gas.By the temperature and N that adjust circulator bath2Flow is adjusted
The concentration of VOC in gas.
Its pressure value is measured by pressure gauge after ball valve BV, filter F in branch 2, subsequently into mass flow control
Device FM metering processed, flowmeter are connect with control instrument, can be precisely controlled flow.Check valve CV is then passed through, gating component is adjusted
SV2 may be selected to enter or do not enter water saturation generator.
Above-mentioned water saturation generator is connected with the second constant temperature circulator 10 through outputting and inputting pipeline, the second constant temperature circulating
In device 10 plus deionized water is circulation fluid, and 0 DEG C~95 DEG C of bath temperature adjustable.The N of certain flow2It flows through in saturation generator
Deionized water carries out the vapor of certain content.By the temperature and N that adjust circulator bath2Flow carrys out water in regulating gas
Content.
Second may be configured as the VOC calibrating gas steel gas cylinder of nitrogen or certain concentration with gas cylinder 8.It, can when being set as nitrogen
As carrier gas, the concentration and reaction velocity of reaction gas are adjusted.When being set as VOC calibrating gas, VOC can be saved and be bubbled step
Suddenly, easy to operate, it is suitble to the measurement of standard curve.Gas in steel cylinder is depressurized through pressure reducing valve, in access device gas circuit, warp
Its pressure value is measured by pressure gauge after ball valve BV, filter F, subsequently into mass flow controller FM measure, flowmeter with
Control instrument connection, can be precisely controlled flow, then pass through check valve CV and third triple valve TV3, with branch 1 and/or branch 2
Gas converges；
After the gas of all branches converges, the 4th triple valve TV4 and the 5th triple valve TV5 is adjusted, mixed gas may be selected
It is reacted into reactor 4, or is directly entered chromatograph 6 and is analyzed.After gas enters reactor 4, with the suction in reactor 4
Attached dose of haptoreaction is discharged into gas chromatograph 6 from reactor lower end and analyzes, and the data such as gas component, concentration are by computer 7
Chromatographic work station show that residual gas discharges after entering tail gas absorption bottle 5 by the road from gas chromatograph gas outlet in real time.Instead
Quartz ampoule built in device and open type electric heating reacting furnace are answered, for electric heating reacting furnace by temperature programmed control, instrument is temperature automatically controlled, on quartz ampoule
End connection pressure gauge, middle part is equipped with temperature tube and thermocouple.
A kind of the embodiment of the present invention 2 are as follows: evaluating apparatus progress gas evaluation for escaping gas performance of the adsorbent
Method, with CS2For adsorbent:
(1) adsorbent tabletting to be measured is sieved, be made it is granular after weigh adsorbent and be placed in the quartz ampoule of reactor.
(2) second match gas cylinder 8 for CS2Calibrating gas is opened gas cylinder switch and pressure reducing valve, is led to after ball valve BV, filter F
Excess pressure table measures its pressure value, subsequently into mass flow controller FM, after the instrument on control panel sets flow value
Into gas circuit.
(3) first match gas cylinder 1 for N2, gas cylinder switch and pressure reducing valve are opened, regulating three-way valve TV1, branch 2, which is in, closes
State, gas enter branch 1, its pressure value are measured by pressure gauge after ball valve BV, filter F, subsequently into quality stream
Amount controller FM can be precisely controlled flow, then pass through check valve CV after the instrument on control panel sets flow value, adjust
Gating component SV1 is saved, gas does not enter VOC saturation generator, only as the carrier gas of calibrating gas, adjusts the second triple valve
TV2 and third triple valve TV3, makes branch gas mixing.When room temperature is too low, the pipeline that mixed gas is passed through is opened heating tape and is added
Heat prevents from condensing.
(4) the 5th triple valve TV5 before the 4th triple valve TV4 and gas chromatograph 6 before adjusting reactor 4, so that one
Determine the CS of concentration2Mixed gas directly passes through pipeline and enters gas chromatograph 6, the concentration before analyzing reaction, then by piping connection
It is discharged after to tail gas absorption bottle 5.
(5) the 5th threeway before the 4th triple valve TV4 and gas chromatograph 6 after concentration is stablized, before adjusting reactor 4
Valve TV5, so that certain density CS2Mixed gas enters in reactor 4, is discharged from 4 lower end of reactor, into gas-chromatography
It is analyzed in instrument 6.
(6) it after to be penetrated, shuts down procedure, arranges data measured, residual gas is by piping connection to 5 heel row of tail gas absorption bottle
It puts.
(7) change the heating temperature of reactor to set desorption temperature, adjust N2Flow carries out detachment assays, and gas is desorbed
Body enters the detection of gas chromatograph 5.
(8) by changing calibrating gas component, concentration, reacting furnace temperature etc., multiple groups experiment test is carried out, experiment is improved
Efficiency.According to the data measured, the working curve of surveyed adsorbent is obtained, judge absorption/desorption ability of adsorbent.
The embodiment of the present invention 3 are as follows: a kind of evaluating apparatus for escaping gas performance of the adsorbent carries out water in gas
The evaluation method that the content of steam influences performance of the adsorbent, with CS2For adsorbent:
The present embodiment and implementation 2 are not both to adjust the first triple valve TV1, and branch 2 is in the open state, adjusts gating group
Part SV2, gas enter water saturation generator 3.Specifically, the N in branch 22Pass through pressure gauge after ball valve BV, filter F
Its pressure value is measured, can precisely be controlled after the instrument on control panel sets flow value subsequently into mass flow controller FM
Flow processed then passes through check valve CV, adjusts gating component SV2, and gas enters water saturation generator 3, carries a certain amount of water
Steam enters mixed pipe line, and the bath temperature of the second constant temperature circulator 10 is set within the scope of 0 DEG C~95 DEG C, adjusts N2Flow,
To regulate and control the content into the vapor in gas circuit, other parameters are same as Example 1.By change calibrating gas component,
Concentration, reacting furnace temperature, water vapour content etc. carry out multiple groups experiment test, improve conventional efficient.According to the data measured,
The working curve for obtaining surveyed adsorbent judges absorption/desorption ability influence of the water vapour content to adsorbent.
A kind of the embodiment of the present invention 4 are as follows: evaluating apparatus progress gas evaluation for escaping gas performance of the adsorbent
Method:
The present embodiment is not both that second closes with gas cylinder 8 connect gas circuit with implementing 3, adjust gating component SV1 with
SV2 makes the N in branch 12N into VOC saturation generator 2, in branch 22Gas does not enter water saturation generator 3.Specifically,
N in branch 12Its pressure value is measured by pressure gauge after ball valve BV, filter F, subsequently into mass flow controller
FM can be precisely controlled flow after the instrument on control panel sets flow value, then pass through check valve CV, adjust gating group
Part SV1, gas enter VOC saturation generator.N in branch 22Its pressure is measured by pressure gauge after ball valve BV, filter F
Force value can be precisely controlled flow after the instrument on control panel sets flow value subsequently into mass flow controller FM,
Check valve CV is then passed through, gating component SV2 is adjusted, gas does not enter water saturation generator 3, carrier gas is only used as, after mixing
Reaction gas is formulated as various concentration.The temperature of the first constant temperature circulator 9 is set within the scope of -5 DEG C~95 DEG C, adjusts N2's
Flow, to regulate and control into the VOC gas concentration in gas circuit.Other parameters are identical as embodiment 2.It can be mixed by changing VOC
Gas concentration, temperature of reactor etc. are closed, multiple groups experiment test is carried out, improves conventional efficient.According to the data measured, institute is obtained
The working curve for surveying adsorbent, judges absorption/desorption ability influence of the factors pair such as VOC concentration.
Claims (10)
1. a kind of evaluating apparatus for escaping gas performance of the adsorbent, including gas absorption/desorption system and on-line analysis
Display system, which is characterized in that
Gas absorption/the desorption system includes first matching gas cylinder (1), first with gas cylinder (1) through the first triple valve (TV1) by gas
Body is divided into two branches, and branch 1 is connect by the first gating component (SV1) with VOC saturation generator (2), and branch 2 passes through the second choosing
Logical component (SV2) is connect with water saturation generator (3), and VOC saturation generator (2) and water saturation generator (3) outlet conduit are logical
Cross after the second triple valve (TV2) converges, through the 4th triple valve (TV4) and the 5th triple valve (TV5) respectively with reactor (4) and
The connection of line analysis display system, reactor outlet are connect through the 5th triple valve (TV5) with on-line analysis display system, then by pipeline
It is connected to tail gas absorption bottle (5)；
The on-line analysis display system includes gas chromatographicanalyzer (6) and computer (7), and the two is connected by Serial Port Line, gas
Analysis of hplc instrument (6) and reactor (4) outlet connect.
2. the apparatus according to claim 1, which is characterized in that the gas absorption/desorption system further includes the second distribution
Bottle (8), second is converged with gas cylinder (8) by third triple valve (TV3) and branch 1 and/or 2 gas of branch.
3. the apparatus according to claim 1, which is characterized in that first gating component (SV1) and the second gating component
(SV2) it is the two sets of ball valves being set side by side, wherein one group of ball valve is two concatenated ball valves, connects VOC between two ball valves
Saturation generator (2) or water saturation generator (3), another group of ball valve are a ball valve, both ends respectively with VOC saturation generator
(2) or the connection of the inlet and outlet of water saturation generator (3), gas occur by the way that after gating component, selectivity is saturated into VOC
Device (2) or water saturation generator (3).
4. the apparatus according to claim 1, which is characterized in that the VOC saturation generator (2) and the first constant temperature circulator
(9) it is output and input pipeline to be connected, deionized water is added in first constant temperature circulator (9) or dehydrated alcohol is circulation fluid,
Bath temperature is -5 DEG C~95 DEG C；The water saturation generator (3) and the second constant temperature circulator (10) are through outputting and inputting pipeline
It is connected, in second constant temperature circulator (10) plus deionized water is circulation fluid, and bath temperature is 0 DEG C~95 DEG C.
5. the apparatus according to claim 1, which is characterized in that quartz ampoule and open type electric heating built in the reactor (4)
Reacting furnace, upper end connection are located at the pressure gauge outside reactor, and lower end connection is located at the electric thermo-couple temperature induction outside reactor
Device and temperature control panel.
6. the apparatus of claim 2, which is characterized in that described first matches gas cylinder (1) for nitrogen steel gas cylinder, and second matches
Gas cylinder (8) is the VOC calibrating gas steel gas cylinder of nitrogen or certain concentration；Described first goes out with gas cylinder (1) and second with gas cylinder (8)
Mouth connection pressure reducing valve.
7. the apparatus of claim 2, which is characterized in that the branch 1, branch 2 and second are matched on gas cylinder pipeline, edge
Gas flow direction is successively arranged ball valve (BV), filter (F), mass flowmenter (FM) and check valve (CV), the filter
It is connect with pressure gauge, the flowmeter is connect with control instrument, for being precisely controlled flow.
8. the evaluation method of escaping gas performance of the adsorbent evaluating apparatus is used for described in any one of claim 1-7, it is special
Sign is to include the following steps:
(1) adsorbent tabletting to be measured is sieved, the adsorbent of certain partial size is made, weighs a certain amount of adsorbent and is placed in reactor
Quartz ampoule in；
(2) first are set as nitrogen with gas cylinder (1), adjust the first triple valve (TV1), and gas is divided into all the way or two branches,
Wherein, the first gating component (SV1) is adjusted, 1 gas-selectively of branch enters VOC saturation generator (2)；Adjust the second gating group
Part (SV2), 2 gas-selectively of branch enter water saturation generator (3)；The second triple valve (TV2) is adjusted, branch 1 and branch 2 are made
Gas converges；
(3) the second VOC standard for being set as nitrogen or certain concentration with gas cylinder (8) with bottle with gas cylinder (8) or by second is closed
Gas, wherein when being set as the VOC calibrating gas of nitrogen or certain concentration, adjust third triple valve (TV3), make itself and branch 1
And/or 2 gas of branch converges；
(4) after the gas of all branches converges, before the 4th triple valve (TV4) and gas chromatograph (6) before adjusting reactor (4)
The 5th triple valve (TV5), make mixed gas selectively enter reactor (4) reaction or be directly entered gas chromatograph (6) into
Row analysis, wherein after gas enters reactor (4), with the adsorbent haptoreaction in reactor (4), arranged from reactor lower end
Out, into chromatographic (6), residual gas enters tail gas absorption bottle (5) from gas chromatograph (6) gas outlet by the road
After discharge；
(5) it according to the data measured, obtains the working curve of surveyed adsorbent, judges absorption/desorption ability of adsorbent.
9. evaluation method according to claim 8, which is characterized in that in the step (2) VOC saturation generator (2) with
First constant temperature circulator (9) is output and input pipeline and is connected, and deionized water or anhydrous is added in first constant temperature circulator (9)
Ethyl alcohol is circulation fluid, and bath temperature is -5 DEG C~95 DEG C；Water saturation generator (3) and the second constant temperature circulator (10) through input and
Output pipe is connected, and in second constant temperature circulator (10) plus deionized water is circulation fluid, and bath temperature is 0 DEG C~95 DEG C；
Reactor (4) is by temperature programmed control in the step (4), for temperature of reactor to be arranged.
10. evaluation method according to claim 8, which is characterized in that in the step (2) and step (3), branch 1, branch
Road 2 and second is successively arranged ball valve (BV), filter (F), mass flowmenter along gas flow direction on gas cylinder (8) pipeline
(FM) connect with check valve (CV), the filter (F) with pressure gauge, for measuring pressure, the mass flowmenter (FM) with
Control instrument connection, for being precisely controlled flow.
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