CN207937473U - A kind of device of on-line monitoring early warning anaerobic fermentation process - Google Patents
A kind of device of on-line monitoring early warning anaerobic fermentation process Download PDFInfo
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- 238000012544 monitoring process Methods 0.000 title claims abstract description 25
- 239000000523 sample Substances 0.000 claims abstract description 120
- 238000012545 processing Methods 0.000 claims abstract description 87
- 239000002253 acid Substances 0.000 claims abstract description 71
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- 239000002699 waste material Substances 0.000 description 16
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 13
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 13
- 238000005086 pumping Methods 0.000 description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 12
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 12
- 239000012153 distilled water Substances 0.000 description 11
- 235000011121 sodium hydroxide Nutrition 0.000 description 11
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 10
- 235000002639 sodium chloride Nutrition 0.000 description 10
- 230000004044 response Effects 0.000 description 8
- 238000004448 titration Methods 0.000 description 7
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 6
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 6
- 239000001110 calcium chloride Substances 0.000 description 6
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- 235000015165 citric acid Nutrition 0.000 description 6
- 238000007405 data analysis Methods 0.000 description 6
- 235000011167 hydrochloric acid Nutrition 0.000 description 6
- 229910000403 monosodium phosphate Inorganic materials 0.000 description 6
- 235000019799 monosodium phosphate Nutrition 0.000 description 6
- 235000011007 phosphoric acid Nutrition 0.000 description 6
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 description 6
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 5
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 5
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 5
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 5
- 235000011130 ammonium sulphate Nutrition 0.000 description 5
- 235000019253 formic acid Nutrition 0.000 description 5
- 239000012071 phase Substances 0.000 description 5
- 239000012488 sample solution Substances 0.000 description 5
- 239000011780 sodium chloride Substances 0.000 description 5
- 235000011148 calcium chloride Nutrition 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 238000002347 injection Methods 0.000 description 4
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- 235000006408 oxalic acid Nutrition 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
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- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
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- 230000005611 electricity Effects 0.000 description 2
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- KQNPFQTWMSNSAP-UHFFFAOYSA-N isobutyric acid Chemical compound CC(C)C(O)=O KQNPFQTWMSNSAP-UHFFFAOYSA-N 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
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- 150000007513 acids Chemical class 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- GWYFCOCPABKNJV-UHFFFAOYSA-N beta-methyl-butyric acid Natural products CC(C)CC(O)=O GWYFCOCPABKNJV-UHFFFAOYSA-N 0.000 description 1
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Landscapes
- Sampling And Sample Adjustment (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The utility model discloses a kind of devices of on-line monitoring early warning anaerobic fermentation process, and device includes sample collection system, sample processing system, adding of agent system, gas collection and sampling system, data collecting system and automatic control system；The sample collection system and adding of agent system are communicated to sample processing system by pipeline respectively；The sample processing system is sequentially connected gas collection by pipeline and is connect with sampling system and data collecting system；The operation that the automatic control system passes through data transmission line traffic control sample collection system, sample processing system, adding of agent system, gas collection and sampling system and each component of data collecting system.The device is combined the way of distillation with gas chromatography, it realizes distillation gas chromatography and carries out online volatile acid detection, it is inaccurate to avoid way of distillation result, the shortcomings of chromatography tedious steps, and the variation of each component content in the variation of volatile acid total amount and volatile acid in anaerobic fermentation can be monitored.
Description
Technical field
The utility model belongs to on-line early warning system and device field, more particularly, to a kind of on-line monitoring early warning anaerobic fermentation
The device of process.
Background technology
Anaerobic fermentation is a kind of effective technology for handling debirs while producing biogas of environmental protection, is led in organic waste
Domain is widely applied.However, the operation stability of anaerobic fermentation process is frequently subjected to the influence of several factors, it is such as feed stock
When matter, influent load, hydraulic retention etc..When these factors change, Hydrolysis Acidification and the methane phase process of fermentation are held
Easily fluctuation or unbalance, causes rancid generation.For example, when influent load is excessively high, organic matter is hydrolyzed production acid in a short time
Bacterium is degraded, and the organic acid of generation cannot be decomposed by methanogen in time, and acid can be caused to inhibit even rancid phenomenon, eventually lead to and detest
Aerobe fermentation system unstability.Therefore, the success or failure that on-line monitoring early warning decides anaerobic fermentation system operation are carried out to anaerobic fermentation.
Volatile acid or volatile fatty acid (VFA), are the intermediate products generated in anaerobic fermentation process.By to waving
The monitoring for the amount of turning sour can directly, fast and accurately react the quality of anaerobic fermentation process, be the best finger that early warning is monitored online
Mark.The not only variation of volatile acid total amount can react anaerobic fermentation state well, and in volatile acid various constituent contents ratio
Example also has much relations with anaerobic fermentation.Such as：The higher bionethanation system of volatile acid total concentration, if acetic acid content account for it is very high
Ratio illustrates that system operation is normal；But isobutyric acid, isovaleric acid illustrate that system loading is excessively high when accounting for very high proportion, need in time
Adjustment.There are many Ahring, Hill and Bolte etc., and scholar's height emphasizes volatile fatty acid each group in monitoring anaerobic fermentation process
Divide the importance of content.Therefore, anaerobic fermentation monitoring technology not only wants the variation of volatile acid total amount during monitor fermentation, also wants
Monitor the variation of each component in volatile acid.
Currently, volatile acid is often divided into detection method：Titration, the way of distillation, colorimetric method, gas chromatography.
Titration：It is directly titrated with soda acid, terminal is judged by pH value variation, is calculated and is volatilized according to acid and alkali consumption amount
Acid content.The disadvantage is that not being suitable for solid content height and the strong situation of buffer capacity, and each component in volatile acid cannot be measured and contained
Amount.
The way of distillation：Volatilization acid distillation is condensed, indicator is then added, with alkali-titration, is waved according to alkali lye consumption calculating
It turns sour content.The disadvantage is that need artificially to judge that terminal, human factor are affected according to color change, it is as a result inaccurate, and not
Each component content in volatile acid can be measured.
Colorimetric method：It is directly added into medicament and complex compound is generated by chemical reaction, then utilize spectrophotometric colo, according to
Standard curve finds out volatile acid content.The disadvantage is that the case where not being suitable for high chroma, and each component in volatile acid cannot be measured
Content.
Gas chromatography：Volatile acid total amount is not only detected using gas chromatograph, but also can be detected each component VFA and be contained
Amount.
Titration, the way of distillation and colorimetric method can only all monitor volatile fatty acid total amount, cannot monitor each constituent content
Variation.Only could monitor the variation of volatile fatty acid each component using gas chromatography at present, it is known that gas-chromatography
Monitoring method is largely offline inspection, and staff is needed first to centrifuge, and phosphorate low-kappa number sample, then recycles gas phase color
Spectrometer detects.
Currently, Chinese patent CN103364523A discloses a kind of volatile acid online monitoring system, which includes extraction
Distribution system, drop reaction device, adding of agent system and automatic control system.The apparatus system can be realized by online titration
Prosthetic is monitored online, but since it cannot measure each component changes of contents in volatile acid, causes early warning inaccurate, may
Lead to error in judgement；In addition, online titration cannot make the anaerobic fermentation of Gao Hangu, high chroma or high buffer capacity
With limitation is larger；So in order to carry out early warning to anaerobic fermentation more extensively, more accurately, it is necessary to which developing can be accurately
Monitor the anaerobic fermentation on-line early warning device of volatile acid total amount and each component changes of contents in real time.
Currently, the method that the laboratory stage announced monitors independent Volatile fatty acid contents on-line is also all based on gas
Then chromatography (GC), Slater etc. are supervised by changing injection orifice using the solid impurity in fluidized bed filter sample with GC
It surveys；Zumbusch etc. handles sample by increasing ultrafiltration system in the front ends GC, to realize on-line monitoring.But filtration method can not be kept away
The problem exempted from is exactly to block, is hardened.This will seriously affect the service life of the accuracy and monitoring device of on-line monitoring.
Head space chromatography of gases (HSGC) utilizes the thought that the way of distillation is combined with gas chromatography, and avoiding filtering, this is difficult
Topic, realizes volatile fatty acid and more accurately monitors, but headspace gas chromatography instrument still needs manual sampling.It not yet sends out at present
It now can be with the headspace gas chromatography of online auto monitoring.The utility model is to be referred from headspace gas chromatography instrument, has invented one kind
The device of early warning anaerobic fermentation is monitored online.
Utility model content
The technical problem to be solved by the present invention is to provide a kind of devices of on-line monitoring early warning anaerobic fermentation process；It should
Device is that the way of distillation is combined with gas chromatography, realizes distillation-gas chromatography and carries out online volatile acid detection, that is, keeps away
It is inaccurate to have exempted from the follow-up titration results of the way of distillation, the shortcomings of the tedious steps of chromatography artificial sample preparation early period, and anaerobism hair can have been monitored
The variation of volatile acid total amount variation and each component content in volatile acid, more accurate to anaerobic fermentation system early warning in ferment.
In order to solve the above technical problems, the utility model adopts the following technical scheme：
A kind of device of on-line monitoring early warning anaerobic fermentation process, including sample collection system, sample processing system, medicament
Dosing system, gas collection and sampling system, data collecting system and automatic control system；The sample collection system and medicament
Dosing system is communicated to sample processing system by pipeline respectively；The sample processing system is sequentially connected gas by pipeline and receives
Collection and sampling system and data collecting system；The automatic control system passes through data transmission line traffic control sample collection system, sample
The operation of product processing system, adding of agent system, gas collection and sampling system and each component of data collecting system.
As being further improved for technical solution, the sample collection system includes：First Unidirectional solenoid valve, first wriggle
Pump pump, the second peristaltic pump and distillation water pot；Anaerobic fermentation tank by pipeline successively with the first Unidirectional solenoid valve, the first peristaltic pump and
The reactive tank connection of sample processing system communicates；The distillation water pot by pipeline successively with the second peristaltic pump and sample treatment system
The reactive tank connection of system communicates.
As being further improved for technical solution, the sample processing system include reactive tank, heater, blender,
Line temperature sensor, online pH meter and acidproof solenoid valve；The heater can be heating mantle, heating rod or heater strip
Deng；The blender can be mechanical agitator, can also be magnetic stirring apparatus；The reactive tank is placed in closed incubator
It is interior；The line temperature sensor and online pH meter are placed in reactive tank；Reactive tank by pipeline be connected to gas collection with
Sampling system, the pipeline connected between reactive tank and gas collection and sampling system are equipped with third solenoid valve, the acidproof electricity
Magnet valve setting is in the logical external world in reactive tank lower part；The volatilization acid gas evaporated enters gas collection and sample introduction by third solenoid valve
System.
As being further improved for technical solution, the adding of agent system include acid solution tank, salt flow container, alkali liquid tank,
First acid metering pump, the second acid metering pump and third lye metering pump；The acid solution tank is sour with first successively by pipeline
Formula metering pump is connected with the reactive tank of sample processing system and is communicated；The salt flow container by pipeline successively with the second acid metering pump
Connected with the reactive tank of sample processing system communicate the alkali liquid tank by pipeline successively at third lye metering pump and sample
The connection of reason system communicates.
As being further improved for technical solution, the gas collection and sampling system include without friction glass syringe,
Stepper motor, third solenoid valve, the 4th Unidirectional solenoid valve and the 5th solenoid valve；Third solenoid valve distills out sample processing system
Gas collection to without friction glass syringe in, the step motor control without friction glass syringe internal gas is passed through
5th solenoid valve is injected into data collecting system, and the 4th Unidirectional solenoid valve is connected to extraneous by wind turbine.
As being further improved for technical solution, the data collecting system includes gas chromatograph；The gas-chromatography
The content of volatile fatty acid each component, detection data are analyzed by automatic control system and are stored up in the gas that instrument detection evaporates
It deposits.
As being further improved for technical solution, the automatic control system includes data processing and transmission unit and can
Programmable controller；Control program and calculation procedure needed for measurement process are set in programmable controller, defeated in measurement process
Enter signal and input programmable controller through data processing and transmission unit, the actuating signal of programmable controller through data processing with
Transmission unit is exported to each action component.
By the device of above-mentioned on-line monitoring early warning anaerobic fermentation process for volatile acid in on-line measurement anaerobic fermentation process
Content.
The monitoring method of the device of the above-mentioned on-line monitoring early warning anaerobic fermentation process of the utility model, includes the following steps：
1) sample collection：According to default, the first peristaltic pump pumps reaction of the 20-40mL samples to sample processing system
In slot, after obtaining testing liquid, automatic control system sends out instruction to adding of agent system；
2) medicament adds：First acid metering pump startup of adding of agent system, pumping 2-4mL phosphoric acid, formic acid, oxalic acid,
Hydrochloric acid or citric acid solution enter in the reactive tank of sample processing system, and 3.0 or less are required to meet pH value；Then adding of agent
The acid metering pump startup of the second of system, pumping 1-2mL niter cakes, sodium chloride, calcium chloride, sodium dihydrogen phosphate or ammonium sulfate are molten
Liquid enters in the reactive tank of sample processing system, reduces the solubility of volatile fatty acid in sample solution；The phosphoric acid, first
A concentration of mass fraction 20%-50% of acid, oxalic acid, hydrochloric acid or citric acid solution；The niter cake sodium chloride, calcium chloride,
A concentration of mass fraction 40%-70 of sodium dihydrogen phosphate or ammonium sulfate；
3) heating stirring：Simultaneously, blender starts to start stirring the acid metering pump startup of the first of adding of agent system；Medicine
The acid metering pump startup of the second of agent dosing system while heater, which start to start, to be heated, 5 DEG C/min of the first stage rate of heat addition,
Heating 7 minutes, 2 DEG C/min of the second stage rate of heat addition, temperature is increased to 100 DEG C of heating and stops, when then temperature drops to 80 DEG C
Heater is again started up, and maintains 75 DEG C of temperature or more at least 2 minutes；
4) sample feeding：For sample processing system temperature at 75 DEG C or more after 2 minutes, automatic control system controls gas collection
Start with the stepper motor propeller of sampling system, slowly without the gas injection data acquisition stored in friction glass syringe
System；
5) sample data acquires：After data collecting system receives sample, gas chromatograph is started to work, and analyzes gaseous sample
Middle volatile fatty acid each component content, and signal response results are sent to automatic control system；
6) data analysis and storage：The data processing of automatic control system receives gas chromatograph response with transmission unit
After signal, programmable controller calculates volatile fatty acid each component content data according to program analysis, and stores to specified
File；
7) reactive tank cleans：After sample introduction, automatic control system controls the second acidproof solenoid valve and the 4th unidirectional electromagnetism
Valve is opened, and wind turbine starts the waste liquid in discharge sample processing system reactive tank, after discharge, the 4th Unidirectional solenoid valve and second acidproof
Solenoid valve is closed；Then the second wriggling pump startup pumps in 80mL distilled water to sample processing system reactive tank, the after two minutes
Four Unidirectional solenoid valves and the second acidproof solenoid valve are opened, the waste liquid in wind turbine startup discharge sample processing system reactive tank, and the 4th
Unidirectional solenoid valve and the second acidproof solenoid valve are closed；Then the second wriggling pump startup, pumping 70mL distilled water to sample treatment system
It unites in reactive tank, third formula measures pump startup, and pumping 2-4mL sodium hydroxides, potassium hydroxide or triethanolamine solution enter sample
In processing system reactive tank, it is anti-to start discharge sample processing system for the 4th Unidirectional solenoid valve and the second acidproof solenoid valve after two minutes
Waste liquid in slot, the 4th Unidirectional solenoid valve and the second acidproof solenoid valve is answered to close；Then the second wriggling pump startup, pumping 80mL distillations
In water to sample processing system reactive tank, the 4th Unidirectional solenoid valve and the second acidproof solenoid valve are opened after two minutes, and wind turbine starts
The waste liquid in sample processing system reactive tank is discharged, the 4th Unidirectional solenoid valve and the second acidproof solenoid valve are closed；The second last is compacted
Dynamic pump startup pumps in 80mL distilled water to sample processing system reactive tank, the 4th Unidirectional solenoid valve and second resistance to after two minutes
Sour solenoid valve is opened, and wind turbine starts the waste liquid in discharge sample processing system reactive tank, the 4th Unidirectional solenoid valve and second acidproof
Solenoid valve is closed；It is standby in case next measurement；A concentration of quality of the sodium hydroxide, potassium hydroxide or triethanolamine solution point
Number 20%-50%；
8) gas piping cleans：Sample processing system, data collecting system after hours, the 4th Unidirectional solenoid valve and
Five solenoid valves are opened, and gas-heating apparatus is opened, and wind turbine is blown to without friction glass syringe, gas chromatograph, stripping pipeline
Interior liquid and impurity etc., 2 minutes duration, then wind turbine stopping, the 4th Unidirectional solenoid valve and the 5th solenoid valve are closed,
It is standby in case next measurement.
Compared with prior art, the utility model has the advantages that：
The volatile acid monitoring range of the on-line early warning device of the utility model is 10-10000mg/L, and single measurement takes
30-40 minutes.Compared to existing measurement means, the utility model realizes the continuous measurement of volatile acid content, and can be in time
Work information is provided to central control room, time of measuring is shortened, saves manpower and materials；The utility model monitored results are accurate
Really, precision is high, can not only monitor the variation of volatile acid total amount, moreover it is possible to monitor each component situation of change in volatile acid；The utility model
It is applied widely, the high anaerobic fermentation system of solid content can not only be monitored, moreover it is possible to monitor the high anaerobic fermentation system of coloration.
Description of the drawings
Specific embodiment of the present utility model is described in further detail below in conjunction with the accompanying drawings
Fig. 1 is the structural schematic diagram for the device that early warning anaerobic fermentation process is monitored online；
Fig. 2 is application on site of the utility model device in the CSTR bioreactors of laboratory scale.
Numeral mark meaning involved in figure is as follows：
The first peristaltic pumps of 12-, 13- distillations water pot, the first Unidirectional solenoid valves of 14-, the second peristaltic pumps of 15-；21- acid solutions tank,
22- salt flow container, 23- alkali liquid tanks, 24- third alkali formulas metering pump, the second acids of 25- metering pump, 26- the first acid metering pumps；32-
Reactive tank, 33- blenders, 34- line temperature sensors, the online pH meters of 35-, the acidproof solenoid valves of 36-, 37- heaters；42- is walked
Stepper motor, 43- thirds solenoid valve, the 4th Unidirectional solenoid valves of 44-, the 5th solenoid valves of 45-, 46- wind turbines, 47- are without friction glass note
Emitter；52- gas chromatographs；62- programmable controllers, 63- data processings and transmission unit；72- incubators.
Specific implementation mode
In order to illustrate more clearly of the utility model, the utility model is done further with reference to preferred embodiment
It is bright.It will be appreciated by those skilled in the art that specifically described content is illustrative and be not restrictive below, it should not be with this
Limit the scope of protection of the utility model.
A kind of device of on-line monitoring early warning anaerobic fermentation process, including sample collection system, sample processing system, medicament
Dosing system, gas collection and sampling system, data collecting system and automatic control system；The sample collection system and medicament
Dosing system is communicated to sample processing system by pipeline respectively；The sample processing system is sequentially connected gas by pipeline and receives
Collection and sampling system and data collecting system；The automatic control system passes through data transmission line traffic control sample collection system, sample
The operation of product processing system, adding of agent system, gas collection and sampling system and each component of data collecting system.
In the preferred embodiment of the utility model, the sample collection system includes：First Unidirectional solenoid valve 14, first
Peristaltic pump 12, the second peristaltic pump 15 and distillation water pot 13；Anaerobic fermentation tank by pipeline successively with the first Unidirectional solenoid valve 14,
The connection of the reactive tank 32 of one peristaltic pump 12 and sample processing system communicates；The distillation water pot 13 is compacted with second successively by pipeline
The connection of reactive tank 32 of dynamic pump 15 and sample processing system communicates.
In the preferred embodiment of the utility model, the sample processing system includes reactive tank 32, heater 37, stirs
Mix device 33, line temperature sensor 34, online pH meter 35 and acidproof solenoid valve 36；The heater 37 can be heating mantle, add
Hot pin or heater strip etc.；The blender can be mechanical agitator, can also be magnetic stirring apparatus；The reactive tank 32 is set
In in closed incubator 72；The line temperature sensor 34 and online pH meter 35 are placed in reactive tank 32；Reactive tank 32
It is connected to gas collection and sampling system by pipeline, is connected on the pipeline between reactive tank 32 and gas collection and sampling system
Equipped with third solenoid valve 43, the setting of acidproof solenoid valve 36 is in the logical external world in 32 lower part of reactive tank.The volatilization acid gas evaporated
Enter gas collection and sampling system by third solenoid valve 43.
In the preferred embodiment of the utility model, the adding of agent system includes acid solution tank 21, salt flow container 22, alkali
Flow container 23, the first acid metering pump 26, the second acid metering pump 25 and third lye metering pump 24；The acid solution tank 21 passes through pipe
Road connect with the reactive tank 32 of the first acid metering pump 26 and sample processing system communicate successively；The salt flow container 22 passes through pipeline
Connect and communicate with the reactive tank 32 of the second acid metering pump 25 and sample processing system successively, the lye 23 by pipeline successively
It connect and communicates with third lye metering pump 24 and sample processing system.
In the preferred embodiment of the utility model, the gas collection includes without friction glass syringe with sampling system
47, stepper motor 42, third solenoid valve 43, the 4th Unidirectional solenoid valve 44 and the 5th solenoid valve 45；Third solenoid valve 43 is by sample
The gas collection that processing system distills out is in without friction glass syringe 47, and the control of the stepper motor 42 is without friction glass note
Internal gas is injected into data collecting system by emitter 47 by the 5th solenoid valve 45, and the 4th Unidirectional solenoid valve 44 passes through wind turbine 46
Connection is extraneous.
In the preferred embodiment of the utility model, the data collecting system includes gas chromatograph 52；The gas phase
Chromatograph 52 detects the content of volatile fatty acid each component in the gas evaporated, and detection data passes through automatic control system point
Analysis storage.
In the preferred embodiment of the utility model, the automatic control system includes data processing and transmission unit 63
With programmable controller 62；Control program and calculation procedure needed for measurement process are set in programmable controller 62, measure
Input signal in journey inputs programmable controller 62, the action letter of programmable controller 62 through data processing and transmission unit 63
It number is exported to each action component through data processing and transmission unit 63.
By the device of above-mentioned on-line monitoring early warning anaerobic fermentation process for volatile acid in on-line measurement anaerobic fermentation process
Content, include the following steps：
1) sample collection：According to default, it is anti-to sample processing system that the first peristaltic pump 12 pumps 20-40mL samples
It answers in slot 32, after obtaining testing liquid, automatic control system sends out instruction to adding of agent system；
2) medicament adds：The acid metering pump 26 of the first of adding of agent system starts, pumping 2-4mL phosphoric acid, formic acid, grass
Acid, hydrochloric acid or citric acid solution enter in the reactive tank 32 of sample processing system, and 3.0 or less are required to meet pH value；Then medicine
Second acid metering pump 25 of agent dosing system starts, pumping 1-2mL niter cakes, sodium chloride, calcium chloride, sodium dihydrogen phosphate or
Ammonium sulfate enters in the reactive tank 32 of sample processing system, reduces the solubility of volatile fatty acid in sample solution；Institute
State a concentration of mass fraction 20%-50% of phosphoric acid, formic acid, oxalic acid, hydrochloric acid or citric acid solution；The niter cake, chlorination
A concentration of mass fraction 40%-70% of sodium, calcium chloride, sodium dihydrogen phosphate or ammonium sulfate；
3) heating stirring：The acid metering pump 26 of the first of adding of agent system starts simultaneously, and blender 33, which starts to start, to be stirred
It mixes；Heater 37 starts to start heating, first stage heating speed 25 pump startups of the acid metering of the second of adding of agent system simultaneously
5 DEG C/min of rate is heated 7 minutes, 2 DEG C/min of the second stage rate of heat addition, and temperature is increased to 100 DEG C of heating and stops, then temperature
Heater is again started up when dropping to 80 DEG C, maintains 75 DEG C of temperature or more at least 2 minutes；
4) sample feeding：For sample processing system temperature at 75 DEG C or more after 2 minutes, automatic control system controls gas collection
Start with 42 propeller of stepper motor of sampling system, slowly without the gas injection data stored in friction glass syringe 47
Acquisition system；
5) sample data acquires：After data collecting system receives sample, gas chromatograph 52 is started to work, and analyzes gas sample
Volatile fatty acid each component content in product, and signal response results are sent to automatic control system；
6) data analysis and storage：The data processing of automatic control system receives gas chromatograph 52 with transmission unit 63
After response signal, programmable controller 62 calculates volatile fatty acid each component content data according to program analysis, and stores
To specified folder；
7) reactive tank cleans：After sample introduction, the second acidproof solenoid valve of automatic control system control 36 and the 4th unidirectional electricity
Magnet valve 44 is opened, and wind turbine 46 starts the waste liquid in discharge sample processing system reactive tank 32, after discharge, the 4th Unidirectional solenoid valve 44
It is closed with the second acidproof solenoid valve 36；Then the second peristaltic pump 15 starts, and pumping 80mL distilled water to sample processing system reacts
In slot 32, the 4th Unidirectional solenoid valve 44 and the second acidproof solenoid valve 36 are opened after two minutes, and wind turbine starts discharge sample treatment system
The waste liquid united in reactive tank 32, the 4th Unidirectional solenoid valve 44 and the second acidproof solenoid valve 36 are closed；Then the second peristaltic pump 15 opens
It is dynamic, it pumps in 70mL distilled water to sample processing system reactive tank 32, third formula metering pump 24 starts, and pumps 2-4mL hydroxides
Sodium, potassium hydroxide or triethanolamine solution enter in sample processing system reactive tank 32, the 4th Unidirectional solenoid valve 44 after two minutes
Start waste liquid in discharge sample processing system reactive tank 32 with the second acidproof solenoid valve 36, the 4th Unidirectional solenoid valve 44 and second is resistance to
Sour solenoid valve 36 is closed；Then the second peristaltic pump 15 starts, and pumps in 80mL distilled water to sample processing system reactive tank 32, two
The 4th Unidirectional solenoid valve 44 and the second acidproof solenoid valve 36 are opened after minute, and wind turbine starts discharge sample processing system reactive tank 32
Interior waste liquid, the 4th Unidirectional solenoid valve 44 and the second acidproof solenoid valve 36 are closed；The second last peristaltic pump 15 starts, and pumps 80mL
In distilled water to sample processing system reactive tank 32, the 4th Unidirectional solenoid valve 44 and the second acidproof solenoid valve 36 are opened after two minutes
It opens, wind turbine starts the waste liquid in discharge sample processing system reactive tank 32, the 4th Unidirectional solenoid valve 44 and the second acidproof solenoid valve
36 close；It is standby in case next measurement；A concentration of mass fraction of the sodium hydroxide, potassium hydroxide or triethanolamine solution
20%-50%；
8) gas piping cleans：Sample processing system, data collecting system after hours, 44 He of the 4th Unidirectional solenoid valve
5th solenoid valve 45 is opened, and gas-heating apparatus is opened, and wind turbine 46 is blown to without friction glass syringe 47, gas chromatograph 52
Gas, liquid and impurity in stripping pipeline etc., 2 minutes duration, then wind turbine 46 stop, 44 He of the 4th Unidirectional solenoid valve
5th solenoid valve 45 is closed, standby in case next measurement.
The operation principle of the utility model：
1. theoretical foundation：In a closed system, when liquids and gases reach equilibrium state, volatile liquid Pi's
Partial pressure is the steam pressure P of pure solvent in solutioni 0, the molar fraction Xi of pure solvent in solution, and in solution pure solvent activity
Coefficient gammaiA function, obey following formula
Pi=Pi 0Xiγi
If mixture does not influence each other, γi=1, γ in non-ideal liquid solutioniSize depend on solute and solvent.
When the volatile quantity of solute is less than 1%, γiValue be constant, Raoult's law can be reduced to Henry's law, waving in gas phase
The concentration C of hair propertyGThe concentration C being proportional in liquid phaseL, such as following formula：
CG/CL=K
K is distribution coefficient or dimensionless Henry'S coefficient
According to liquid sample volume V under equilibrium stateLWith gas volume VG, the equilibrium concentration C of liquidLLess than initial concentration
CL0, it is assumed that before and after balance, the constancy of volume of liquid phase.
CL0VL=CLVL+CGVG
Or CL0VL+=KCGVL+CGVG
The peak area A of top space measurement is calculated, it is directly proportional to gas phase concentration
If VGAnd VLIt is constant, distribution coefficient is very high, then K>>VG/VL, i.e. K+VG/VL=K, by taking VFA as an example,
Equation (1) can turn to
This is the theoretical foundation of the utility model VFA monitoring systems.
2. principle：Tthe utility model system principle is VFA phase separations in situ, and detects headspace analysis using GC.Step
It is as follows
A) 20-40mL water samples are taken from anaerobic system circulation loop.
B) phosphoric acid, formic acid, oxalic acid, hydrochloric acid or the citric acid solution that 2-4mL mass fractions are 20%-50% is added, simultaneously
Start to stir, makes the pH of sample<3.0.
C) niter cake, sodium chloride, calcium chloride, sodium dihydrogen phosphate or the sulfuric acid of 1-2mL mass fractions 40%-70% is added
Ammonium salt solution starts simultaneously at heating, reduces solubility of the volatile fatty acid in sample solution.
D) heat sample, maintain sample solution temperature 75 DEG C or more at least 2 minutes.
E) gas collection is carried out with without friction glass syringe；Then stepper motor is used to carry out gas sampling.
F) it the gas sampling of acquisition, injects in GC instruments and carries out data analysis
G) it data analysis and stores.
H) sample waste is discharged, and cleaning and flushing device are in case detection next time.
Then the response signal of GC is carried out off-line analysis and calculates each component concentration of VFA in the liquid phase.With it is traditional
Static HSGC methods (total gas volume is constant) are different, which collects gas using variable head space volume, extract in gas
System pressure is kept to be equal to atmospheric pressure during taking.Used system schematic is as shown in Figure 1
Embodiment 1：
The monitoring method of prior-warning device is monitored online in the utility model anaerobic fermentation
Step 1：Sample collection.According to default, the first peristaltic pump pumps 20-40mL samples to sample processing system
Reactive tank in, after obtaining testing liquid, automatic control system sends out instruction to adding of agent system
Step 2：Medicament adds.The acid metering pump startup of adding of agent system first, pumping 2-4mL phosphoric acid, formic acid, grass
Acid, hydrochloric acid or citric acid solution enter in the reactive tank of sample processing system, and 3.0 or less are required to meet pH value；Then medicament
It is the second acid metering pump startup to add, and pumping 1-2mL niter cakes, sodium chloride, calcium chloride, sodium dihydrogen phosphate or ammonium sulfate are molten
Liquid enters in the reactive tank of sample processing system, reduces the solubility of volatile fatty acid in sample solution；
Step 3：Heating stirring.Simultaneously, blender starts to start to be stirred the acid metering pump startup of adding of agent system first
It mixes；Heat pump starts to start heating, 5 DEG C/min of the rate of heat addition, heating 7 the acid metering pump startup of adding of agent system second simultaneously
Minute, then the rate of heat addition is decreased to 2 DEG C/min, maintains 75 DEG C of temperature or more at least 2 minutes.
Step 4：Sample feeding.For sample processing system temperature at 75 DEG C or more after 2 minutes, automatic control system controls gas
Body is collected to be started with sampling system stepper motor propeller, slowly without the gas injection data stored in friction glass syringe
Acquisition system.
Step 5：Sample data acquires.After data collecting system receives sample, gas chromatograph is started to work, and analyzes gas
Volatile fatty acid each component content in body sample, and signal response results are sent to automatic control system.
Step 6：Data analysis and storage.Automatic control system data analysis unit receives gas chromatograph response letter
After number, volatile fatty acid each component content data is calculated according to program analysis, and store to specified folder.
Step 7：Reactive tank cleans.After sample introduction, robot control system(RCS) controls the second acidproof solenoid valve, the 4th unidirectional electromagnetism
Valve open, air blower start discharge sample processing system reactive tank in waste liquid, the 4th, second solenoid valve close；Then second
Wriggling pump startup pumps in 80mL distilled water to sample processing system reactive tank, and the 4th, second solenoid valve is opened after two minutes,
Air blower start discharge sample processing system reactive tank in waste liquid, the 4th, second solenoid valve close；Then the second peristaltic pump opens
It is dynamic, it pumps in 70mL distilled water to sample processing system reactive tank, lye measures pump startup, pumping 2mL sodium hydroxides, hydroxide
Potassium or triethanolamine solution enter in sample processing system reactive tank, and the 4th, second solenoid valve starts discharge sample after two minutes
Waste liquid in processing system reactive tank, the 4th, second solenoid valve close；Then the second wriggling pump startup, pumping 80mL distilled water is extremely
In sample processing system reactive tank, the 4th, second solenoid valve is opened after two minutes, and it is anti-that air blower starts discharge sample processing system
Answer the waste liquid in slot, the 4th, second solenoid valve closes；The second last wriggling pump startup, pumping 80mL distilled water to sample treatment
In system response slot, the 4th, second solenoid valve is opened after two minutes, and air blower starts in discharge sample processing system reactive tank
Waste liquid, the 4th, second solenoid valve close；It is standby in case next measurement.
Step 8：Gas piping cleans.Sample processing system, data collecting system after hours, the 4th solenoid valve,
Five solenoid valves are opened, and gas-heating apparatus is opened, and air blower is to without friction glass syringe, and gas chromatograph is blown afloat, blow-off tube
Liquid and impurity in road etc., 2 minutes duration, then wind turbine stop, fourth, fifth solenoid valve close, it is standby in case under
Secondary measurement.
As shown in Figure 2：The monitoring system of the utility model is connected to the CSTR reactors of a 7.2L, system operation is super
6 months are spent, to monitor the VFA concentration of reactor, and compared with the VFA concentration of the artificial off-line measurements of GC-FID.
Obviously, above-described embodiment of the utility model is only intended to clearly illustrate the utility model example, and
It is not the restriction to the embodiment of the utility model.For those of ordinary skill in the art, in above description
On the basis of can also make other variations or changes in different ways.Here all embodiments can not be exhaustive.
It is every to belong to obvious changes or variations that the technical solution of the utility model is extended out still in the utility model
The row of protection domain.
Claims (7)
1. a kind of device of on-line monitoring early warning anaerobic fermentation process, it is characterised in that：Including sample collection system, sample treatment
System, adding of agent system, gas collection and sampling system, data collecting system and automatic control system；The sample collection
System and adding of agent system are communicated to sample processing system by pipeline respectively；The sample processing system by pipeline successively
Connect gas collection and sampling system and data collecting system；The automatic control system is adopted by data transmission line traffic control sample
The fortune of collecting system, sample processing system, adding of agent system, gas collection and sampling system and each component of data collecting system
Row.
2. the device of early warning anaerobic fermentation process is monitored online according to claim 1, it is characterised in that：The sample collection
System includes：First Unidirectional solenoid valve, the first peristaltic pump, the second peristaltic pump and distillation water pot；Anaerobic fermentation tank by pipeline according to
The secondary reactive tank with the first Unidirectional solenoid valve, the first peristaltic pump and sample processing system, which is connect, to be communicated；The distillation water pot passes through
Pipeline connect with the reactive tank of the second peristaltic pump and sample processing system communicate successively.
3. the device of early warning anaerobic fermentation process is monitored online according to claim 1, it is characterised in that：At the sample
Reason system includes reactive tank, heater, blender, line temperature sensor, online pH meter and acidproof solenoid valve；The heater
Including heating mantle, heating rod or heater strip；The blender includes mechanical agitator or magnetic stirring apparatus；The reactive tank is set
In in closed incubator；The line temperature sensor and online pH meter are placed in reactive tank；Reactive tank is connected by pipeline
It is connected to gas collection and sampling system, the pipeline connected between reactive tank and gas collection and sampling system is equipped with third electromagnetism
Valve, the acidproof solenoid valve setting is in the logical external world in reactive tank lower part；The volatilization acid gas evaporated is entered by third solenoid valve
Gas collection and sampling system.
4. the device of early warning anaerobic fermentation process is monitored online according to claim 1, it is characterised in that：The medicament is thrown
Adding system includes acid solution tank, salt flow container, alkali liquid tank, the first acid metering pump, the second acid metering pump and third lye metering pump；
The acid solution tank is connect successively with the reactive tank of the first acid metering pump and sample processing system by pipeline and is communicated；The saline solution
Tank is connect successively with the reactive tank of the second acid metering pump and sample processing system by pipeline and is communicated；The alkali liquid tank passes through pipe
Road connect with third lye metering pump and sample processing system communicate successively.
5. the device of early warning anaerobic fermentation process is monitored online according to claim 1, it is characterised in that：The gas collection
Include without friction glass syringe, stepper motor, third solenoid valve, the 4th Unidirectional solenoid valve and the 5th electromagnetism with sampling system
Valve；The gas collection that third solenoid valve distills out sample processing system is in without friction glass syringe, the stepper motor
Internal gas is injected into data collecting system, the 4th Unidirectional solenoid valve by control without friction glass syringe by the 5th solenoid valve
It is connected to by wind turbine extraneous.
6. the device of early warning anaerobic fermentation process is monitored online according to claim 1, it is characterised in that：The data acquisition
System includes gas chromatograph；The content of volatile fatty acid each component in the gas that the gas chromatograph detection evaporates,
Detection data is analyzed by automatic control system and is stored.
7. the device of early warning anaerobic fermentation process is monitored online according to claim 1, it is characterised in that：The automatic control
System processed includes data processing and transmission unit and programmable controller；Control program and calculation procedure needed for measurement process are set
Programmable controller is inputted through data processing and transmission unit due to the input signal in programmable controller, measurement process, it can
The actuating signal of programmable controller is exported through data processing and transmission unit to each action component.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109738383A (en) * | 2018-12-14 | 2019-05-10 | 山东大学 | A kind of on-line monitoring equipment and method of volatile fatty acid |
| CN110361551A (en) * | 2018-04-09 | 2019-10-22 | 北京化工大学 | A kind of device and method that early warning anaerobic fermentation process is monitored online |
-
2018
- 2018-04-09 CN CN201820494023.6U patent/CN207937473U/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110361551A (en) * | 2018-04-09 | 2019-10-22 | 北京化工大学 | A kind of device and method that early warning anaerobic fermentation process is monitored online |
| CN109738383A (en) * | 2018-12-14 | 2019-05-10 | 山东大学 | A kind of on-line monitoring equipment and method of volatile fatty acid |
| CN109738383B (en) * | 2018-12-14 | 2020-04-21 | 山东大学 | Online monitoring device and method for volatile fatty acid |
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