CN105021651A - Synchronized quantitative analysis method of biomass combustion and gaseous emission, - Google Patents
Synchronized quantitative analysis method of biomass combustion and gaseous emission, Download PDFInfo
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- CN105021651A CN105021651A CN201510394001.3A CN201510394001A CN105021651A CN 105021651 A CN105021651 A CN 105021651A CN 201510394001 A CN201510394001 A CN 201510394001A CN 105021651 A CN105021651 A CN 105021651A
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Abstract
The present invention discloses a synchronized quantitative analysis method of biomass combustion and gaseous emission. The method comprises the steps of: 1) testing and analyzing a biomass sample in a synchronized thermal analyzer to obtain a combustion characteristic curve; 2) simultaneously introducing the gas produced in the step 1) through connecting pipes into a Fourier transform infrared spectroscopy analyzer and mass spectrometer, testing and analyzing to obtain the gas composition and content. The analysis method can realize rapid on-line monitoring and obtains comprehensive and reliable data. The combined technology makes up for the shortcoming of reorganization failure in overlapping peaks in separate detection by the infrared analyzer, as well as the defect that the mass spectrometer can not detect ions with the same mass to charge ratio; the method has high sensitivity, can effectively improve the analysis and monitoring of efficiency and help cost saving and consumption reduction in biomass straw combustion energy utilization.
Description
Technical field
The invention belongs to analysis and testing technology field, be specifically related to a kind of biomass combustion and the synchronous quantitative analysis method of gas discharging.
Background technology
China is stalk big producing country, can the fully high efficiency stalk resource utilizing China's abundant by stalk direct combustion generating, can alleviate the pressure of fossil resource exhaustion simultaneously.Burning straw, relative to fire coal, has low stain, and its sulphur, nitrogen content are very low, SO in combustion process
2, NO
xdischarge less, in addition to the CO of air
2discharge capacity is approximately equal to zero, effectively can alleviate greenhouse effect.But straw burning process also may produce secondary pollution.Based on above energy situation and the multiple pressure from environmental protection and carbon dioxide discharge-reduction; within 2005, " People's Republic of China's Renewable Energy Law " enacts and enforces; China's Renewable Energy Development is put into the orbit of the legal, advances exploitation and the industry development of regenerative resource effectively.
There are direct combustion power generation, mixed combustion generating and gasifying electricity generation in the major technique path of straw generating technology.The design and running way choice of biomass combustion equipment must from living beings own combustion characteristic, technical, the economy that guarantee runs and reliability.The burning of living beings also unavoidably produces secondary pollution, therefore, implements monitoring analysis also very important to the product row of burn process gases.The thermogravimetry comparative maturity of independent postgraduate's substance combustion characteristic, for the monitoring analysis of burn process gases, existing method adopts single equipment monitoring, obtains data and there is the shortcoming that sensitivity is low, accuracy is low.
Summary of the invention
The object of this invention is to provide a kind of biomass combustion and the synchronous quantitative analysis method of gas discharging.
Analytical approach provided by the present invention, comprises the steps:
1) biomass samples is placed in synchronous solving and carries out test analysis, obtain combustion pattern;
2) by step 1) in produce gas be incorporated in ftir analysis instrument and mass spectrometer by connecting pipe simultaneously, carry out test analysis, learn component and the content of gas.
In above-mentioned analytical approach, step 1) in, described biomass samples specifically can be agricultural crop straw (as: wheat stalk), described biomass samples can prepare by the standard method in test material association of the U.S. (American Society for Testing Material, ASTM).
The mixed gas of nitrogen and oxygen is passed in described synchronous solving, wherein, oxygen purity is 19.5-23.5%, and the flow of described mixed gas specifically can be determined according to instrument and testing requirements, be generally 50-100mL/min, specifically can be 100mL/min.
The condition of described test analysis is as follows:
Be 10-30 DEG C/min by heating rate, be specially 20 DEG C/min) be warming up to 900-1000 DEG C (being specially 1000 DEG C) from room temperature (25 DEG C), obtain combustion pattern.
By biomass samples being placed in the alumina crucible of thermobalance support, the temperature variant whole combustion process of microbalance system record sample quality, thus obtain the combustion pattern of sample.
In above-mentioned analytical approach, step 2) in, described connecting pipe specifically can be quartz capillary.
Step 1) in the gas that produces enter into the special gas pond of ftir analysis instrument, in order to effectively prevent condensation of gas, described connecting pipe and special gas pond are all heated to 150 DEG C.
The test condition of described ftir analysis instrument is as follows:
Resolution is 2-8cm
-1, specifically can be 2cm
-1; Test wavelength scope is 450 ~ 4000cm
-1.
Described mass spectrometric test condition is as follows:
Test pattern is C-SEM, and gas flow is 1 ~ 2sccm, and be 1 ~ 200amu (atomic mass unit atomic mass unit) between molecular weight area, resolution is 0.5 ~ 2.5amu, and operating temperature is 25 ~ 150 DEG C.
Pressure differential between synchronous solving and mass spectrometer (p<10-6mbar) makes step 1) in produce gas (i.e. decomposition product) enter into mass spectrometer, account for the 1%-5% (gas sucks in mass spectrometer by mass spectrometer depended on pressure difference, and soakage is the 1%-5% entering infrared total gas) of gross product amount.Mass spectrometer is sent to record in SEM after being separated by fragment according to mass-to-charge ratio m/e.
The present invention utilizes quality in synchronous solving-ftir analysis instrument-mass spectrometer coupling technique Real-time Obtaining biomass combustion process, heat and produces the dynamic changing data of gas, carries out combustion characteristic analysis and gas produce row and realize real-time quantitative analysis according to data.
Specifically by the weight variation with temperature of thermoanalysis technology Real-Time Monitoring sample, obtain the combustion pattern of sample, obtain ignition temperature, volatile combustion maximum rate, volatile combustion maximum rate corresponding temperature, fixed carbon burning maximum rate, fixed carbon burning maximum rate corresponding temperature, all burnt temperature characteristic parameter further, calculate integrated combustion property index according to above parameter;
For analyzing the composition of its gaseous product in thermal analyses process, infrared spectrum is obtained by coupling Fourier turn infrared instrument, energy-wave number-three dimension temperature the curve map of gas generation and the gas two-dimensional map under determining temperature in whole process can be obtained according to ir data, then the characteristic waves corresponding to characteristic group, judges to generate substance classes;
Coupling mass spectrometer measures the component of material mainly through molecule karyoplasmic ratio again, can accurately measure gaseous component in combustion process, assay products variation with temperature trend, obtain the release strength curve of gas according to different mass-to-charge ratio.
Compared with prior art, the present invention has following beneficial effect:
1) the method can realize quick on-line monitoring.
2) data are comprehensively reliable, coupling technique compensate for infrared spectrometric analyzer detect separately the overlap peak of existence cannot the shortcoming of identification, also make up the defect that mass spectrometer cannot detect mass-to-charge ratio same ion simultaneously.
3) the method is highly sensitive.
4) quantitative research and application can be carried out to gas discharging.
Accompanying drawing explanation
Fig. 1 is test unit of the present invention and analyzes schematic diagram, and wherein, 1 is synchronous solving, and 2 is alumina crucibles, and 3 is connecting pipes, and 4 is Fourier transform infrared spectrometer, and 5 is combination gass, and 6 is mass spectrometers.
Fig. 2 is the combustion pattern of wheat stalk in embodiment 1.
Fig. 3 is the collection of illustrative plates under the three-dimensional collection of illustrative plates and peak temperature that in embodiment 1, wheat stalk burning gases generate.
Fig. 4 is that in embodiment 1, wheat stalk mainly discharges gas intensity with temperature dynamic change curve.
Embodiment
Below by specific embodiment, method of the present invention is described, but the present invention is not limited thereto.
Experimental technique described in following embodiment, if no special instructions, is conventional method; Described reagent and material, if no special instructions, all can obtain from commercial channels.
The synchronous quantitative analysis method of embodiment 1, biomass combustion and gas discharging:
1, data acquisition:
1) experimental provision of the present invention as shown in Figure 1: wherein, and 1 is synchronous solving, and 2 is alumina crucibles, 3 is connecting pipes, and 4 is Fourier transform infrared spectrometer, and 5 is combination gas (nitrogen and oxygen, the content of oxygen in combination gas is 22.2%), 6 is mass spectrometers.
Preparation of samples: Pekinese's wheat stalk will be picked up from according to test material association of the U.S. (American Society forTesting Material, ASTM) relevant criterion method process: after the dry 12h of 105 DEG C of drying boxes, utilize disintegrating machine to carry out fragmentation and obtain fine particle, recycling coal pulverizer grinds 3-5min, screen the sample powder obtained by 60 orders (250 μm) afterwards through sieve shaker, obtain wheat stalk sample to be analyzed.
2) according to the experimental provision in Fig. 1, connect combination gas 5, taking 5.5mg wheat stalk sample to be analyzed is placed in the alumina crucible 2 of thermobalance support, 1000 DEG C are warming up to constant heating rate 20 DEG C/min by room temperature (25 DEG C) according to test design, the airflow rate of combination gas 5 is 100mL/min, by the weight variation with temperature of synchronous solving 1 Real-Time Monitoring sample, obtain the combustion pattern of sample, the composition of its gaseous product in thermal analyses process is analyzed;
3) by connecting pipe 3 by step 2) in the gas that generates to be incorporated in Fourier transform infrared spectrometer 4 in special gas pond simultaneously and to carry out corresponding test in mass spectrometer 6 (specifically synchronous solving 1 can be connected by the quartz capillary heated with mass spectrometer 6), wherein, in order to effectively prevent the condensation of gas generated, pipeline 3 and special gas pond are all heated to 150 DEG C, and Fourier transform infrared spectrometer resolution is set to 2cm
-1, surface sweeping region is 450 ~ 4000cm
-1; Mass spectrometric test pattern is C-SEM, and gas flow is 1 ~ 2sccm, is 1 ~ 200amu between molecular weight area, and resolution is 0.5 ~ 2.5amu, and operating temperature is 25 ~ 150 DEG C.
Judge products of combustion kind by coupling Fourier transformation infrared spectrometer 4, determine functional group,
Again by coupling mass spectrometer 6, measure the component of material mainly through molecule karyoplasmic ratio, can accurately measure gaseous component in combustion process, assay products variation with temperature trend, and carry out quantitative test.
2, data analysis and result as follows:
1) under Different factor level, in straw burning process, family curve as shown in Figure 2.TG curve performance example weight variation with temperature, DTG curve performance sample weight loss speed variation with temperature (i.e. the first order derivative curve of TG curve), the thermal change in DSC curve performance sample combustion process.
Can learn from Fig. 2: the combustion process of wheat stalk can be divided into moisture evaporation, and volatile combustion and fixed carbon burn three primary combustion stages and after-flame stage.
By analysis and arrangement thermogravimetric curve, ignition temperature, volatile combustion maximum rate, volatile combustion maximum rate corresponding temperature, fixed carbon burning maximum rate, fixed carbon burning maximum rate corresponding temperature, all burnt temperature and integrated combustion property index series of features parameter can be obtained, as listed in table 1.
The combustion characteristic parameter of table 1 wheat stalk
2) characteristic waves corresponding to characteristic group, judges to generate substance classes:
Wave number is 900 ~ 1500cm
-1the absorption peak at place is caused by C-H in-plane bending vibration, C-O, C-C skeletal vibration, wave number 2280 ~ 2390cm
-1place is CO
2absorption peak, wave number 2800 ~ 3050cm
-1place is hydro carbons absorption peak, wave number 3480 ~ 3960cm
-1place is H
2o absorption peak.Generate the three-dimensional collection of illustrative plates of gas in combustion process as shown in Figure 3, can learn from Fig. 3: main generation gaseous species is CO
2, H
2o and alkanes gas.
According to TG curve, obtain out peak temperature.Fig. 3 is the absorption infared spectrum that wheat stalk Different factor level goes out peak moment gas, can learn as can be seen from Fig. 3: same factor level contrast, for the volatile combustion stage corresponding to first peak, the air release product at its peak point place is mainly CO
2, have the precipitations such as a small amount of alkanes gas in addition; See the fixed carbon combustion phases corresponding to second peak again, CO
2output much larger than first peak, alkanes gas etc. release less.
3) mass spectrometer record is the mass-to-charge ratio of the gas of the existence in each moment.Select the mass-to-charge ratio of specific gas according to energy intensity, obtain the intensity variation curve of this gas of whole interval according to mass-to-charge ratio.Mass-to-charge ratio is selected as listed in table 2, and gas intensity curve as shown in Figure 4, can be learnt from Fig. 4: wheat stalk burning release CO
2temperature variant trend is strictly corresponding with DTG curve.CO
2start to generate, mainly because Volatile and ambient gas generation combustion reaction generate in the volatile combustion stage; Fixed carbon combustion phases is separated out in a large number, many compared with volatile combustion stage growing amount.NO
xhave precipitation at volatile matter and fixed carbon combustion phases, generation is less.HCl and SO
2mainly separate out in the volatile combustion stage, separate out trace.
Table 2 mass-to-charge ratio is chosen
Claims (5)
1. biomass combustion and the synchronous quantitative analysis method of gas discharging, comprise the steps:
1) biomass samples is placed in synchronous solving and carries out test analysis, obtain combustion pattern;
2) by step 1) in produce gas be incorporated in ftir analysis instrument and mass spectrometer by connecting pipe simultaneously, carry out test analysis, learn component and the content of gas.
2. analytical approach according to claim 1, it is characterized in that: step 1) in, pass into the mixed gas of nitrogen and oxygen in described synchronous solving, wherein, oxygen purity is 19.5-23.5%, and the flow of described mixed gas is 50-100mL/min;
The condition of described test analysis: by heating rate be 10-30 DEG C/min from room temperature to 900-1000 DEG C, obtain combustion pattern.
3. analytical approach according to claim 1 and 2, is characterized in that: step 1) in, described biomass samples is agricultural crop straw.
4. the analytical approach according to any one of claim 1-3, is characterized in that: step 2) in, the test condition of described ftir analysis instrument: resolution is 2-8cm
-1, test wavelength scope is 450 ~ 4000cm
-1;
Described mass spectrometric test condition: test pattern is C-SEM, and gas flow is 1 ~ 2sccm is 1 ~ 200amu between molecular weight area, and resolution is 0.5 ~ 2.5amu, and operating temperature is 25 ~ 150 DEG C.
5. the analytical approach according to any one of claim 1-4, is characterized in that: step 2) in, described connecting pipe is quartz capillary.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107505221A (en) * | 2016-12-27 | 2017-12-22 | 中国科学院工程热物理研究所 | The method for measuring boiler ash content of combustible carbon |
| CN108241001A (en) * | 2016-12-27 | 2018-07-03 | 华润水泥技术研发有限公司 | A kind of coal source tracing method |
| CN109490360A (en) * | 2018-12-29 | 2019-03-19 | 中国科学技术大学 | It is a kind of suitable for large sample amount, more atmosphere can be with differential thermal analysis device |
| CN112986371A (en) * | 2021-02-05 | 2021-06-18 | 中国航发北京航空材料研究院 | Method for rapidly determining degassing process parameters of high-temperature alloy powder |
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| CN2783327Y (en) * | 2005-04-11 | 2006-05-24 | 武汉理工大学 | Comprehensive tester for coal combustion property |
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| CN2783327Y (en) * | 2005-04-11 | 2006-05-24 | 武汉理工大学 | Comprehensive tester for coal combustion property |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107505221A (en) * | 2016-12-27 | 2017-12-22 | 中国科学院工程热物理研究所 | The method for measuring boiler ash content of combustible carbon |
| CN108241001A (en) * | 2016-12-27 | 2018-07-03 | 华润水泥技术研发有限公司 | A kind of coal source tracing method |
| CN109490360A (en) * | 2018-12-29 | 2019-03-19 | 中国科学技术大学 | It is a kind of suitable for large sample amount, more atmosphere can be with differential thermal analysis device |
| CN112986371A (en) * | 2021-02-05 | 2021-06-18 | 中国航发北京航空材料研究院 | Method for rapidly determining degassing process parameters of high-temperature alloy powder |
| CN112986371B (en) * | 2021-02-05 | 2023-08-04 | 中国航发北京航空材料研究院 | Rapid determination method for degassing technological parameters of high-temperature alloy powder |
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Application publication date: 20151104 |