CN105424540A - Testing device for volatilization properties of ammonium bisulfate in coal-fired flue gas - Google Patents
Testing device for volatilization properties of ammonium bisulfate in coal-fired flue gas Download PDFInfo
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- BIGPRXCJEDHCLP-UHFFFAOYSA-N ammonium bisulfate Chemical compound [NH4+].OS([O-])(=O)=O BIGPRXCJEDHCLP-UHFFFAOYSA-N 0.000 title claims abstract description 87
- 238000012360 testing method Methods 0.000 title claims abstract description 34
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 239000003546 flue gas Substances 0.000 title claims abstract description 26
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 55
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 24
- 239000011521 glass Substances 0.000 claims abstract description 20
- 238000005303 weighing Methods 0.000 claims abstract description 15
- 230000008859 change Effects 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 229910001868 water Inorganic materials 0.000 claims description 15
- WYTGDNHDOZPMIW-RCBQFDQVSA-N alstonine Natural products C1=CC2=C3C=CC=CC3=NC2=C2N1C[C@H]1[C@H](C)OC=C(C(=O)OC)[C@H]1C2 WYTGDNHDOZPMIW-RCBQFDQVSA-N 0.000 claims description 12
- 238000009833 condensation Methods 0.000 claims description 10
- 230000005494 condensation Effects 0.000 claims description 10
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 8
- 238000005485 electric heating Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000000605 extraction Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 6
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 238000004255 ion exchange chromatography Methods 0.000 claims description 2
- 238000005260 corrosion Methods 0.000 abstract description 3
- 230000007797 corrosion Effects 0.000 abstract description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- QAOWNCQODCNURD-UHFFFAOYSA-M hydrogensulfate Chemical compound OS([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-M 0.000 abstract description 2
- 238000012544 monitoring process Methods 0.000 abstract description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 8
- 238000000354 decomposition reaction Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 229910021529 ammonia Inorganic materials 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000010881 fly ash Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Chemical compound O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000000809 air pollutant Substances 0.000 description 1
- 231100001243 air pollutant Toxicity 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
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Abstract
一种燃煤烟气中硫酸氢铵挥发特性的测试装置,所述装置包括供氮系统、挥发系统和称量系统,所述挥发系统包括恒温炉、玻璃罩和坩埚,所述恒温炉的一侧通过进气管与供氮系统连接,另一侧设有出气管;所述玻璃罩置于恒温炉内;所述坩埚放置在玻璃罩内,其内部盛放被测试的硫酸氢铵样品;所述称量系统称量硫酸氢铵样品的质量。本发明通过监测硫酸氢铵样品随温度和挥发时间的变化情况得到样品的挥发特性,其测试结果可为燃煤锅炉硫酸氢铵的温度调控提供可靠的理论依据和数据支持,有利于解决硫酸氢铵引起的空预器堵塞和后续设备的腐蚀问题。
A test device for the volatilization characteristics of ammonium bisulfate in coal-fired flue gas, the device includes a nitrogen supply system, a volatilization system and a weighing system, the volatilization system includes a constant temperature furnace, a glass cover and a crucible, one part of the constant temperature furnace One side is connected to the nitrogen supply system through the inlet pipe, and the other side is provided with an outlet pipe; the glass cover is placed in a constant temperature furnace; the crucible is placed in the glass cover, and the ammonium bisulfate sample to be tested is contained in it; The weighing system weighs the quality of the ammonium bisulfate sample. The invention obtains the volatilization characteristics of the sample by monitoring the change of the ammonium bisulfate sample with temperature and volatilization time, and the test results can provide a reliable theoretical basis and data support for the temperature regulation of the ammonium bisulfate in the coal-fired boiler, which is beneficial to solve the problem of hydrogen sulfate Air preheater clogging and subsequent equipment corrosion caused by ammonium.
Description
技术领域 technical field
本发明涉及一种用于测试火电厂燃煤烟气中硫酸氢铵挥发特性的装置,属于燃烧技术领域。 The invention relates to a device for testing the volatilization characteristics of ammonium bisulfate in coal-fired flue gas of a thermal power plant, which belongs to the technical field of combustion.
背景技术 Background technique
为了控制NOx的排放,《火电厂大气污染物排放标准》规定,燃煤电厂中NOx的排放量控制在100mg/m3。SCR和SNCR脱硝技术是以NH3或尿素为还原剂对NOx进行选择性还原,是燃煤电厂减少NOx排放的有效技术。 In order to control the emission of NOx, the "Emission Standard of Air Pollutants for Thermal Power Plants" stipulates that the emission of NOx in coal-fired power plants should be controlled at 100mg/m 3 . SCR and SNCR denitrification technologies use NH3 or urea as the reducing agent to selectively reduce NOx , and are effective technologies for reducing NOx emissions in coal-fired power plants.
SCR和SNCR烟气脱硝过程中,在一定条件下,SO3与出口烟气中未反应的逃逸氨(NH3)及水蒸气可生成硫酸氢铵(NH4HSO4,简称ABS)和硫酸铵((NH4)2SO4,简称AS),二者的产生量取决于NH3和SO3的比例。理论上讲,当NH3/SO3摩尔比大于2时,倾向于生成AS;当NH3/SO3摩尔比小于1时,倾向于生成ABS。 In the process of SCR and SNCR flue gas denitrification, under certain conditions, SO 3 and unreacted escape ammonia (NH 3 ) and water vapor in the outlet flue gas can generate ammonium bisulfate (NH 4 HSO 4 , referred to as ABS) and ammonium sulfate ((NH 4 ) 2 SO 4 , referred to as AS), the production of both depends on the ratio of NH 3 and SO 3 . Theoretically, when the NH 3 /SO 3 molar ratio is greater than 2, AS tends to be formed; when the NH 3 /SO 3 molar ratio is less than 1, ABS tends to be formed.
其可能存在的反应如下: Its possible reactions are as follows:
硫酸氢铵的沸点为350℃,熔点为140℃,具有吸湿性、粘性、腐蚀性,在不同的温度下分别呈现气态、液态、颗粒状。气态或颗粒状的硫酸氢铵会随烟气流动,而液态的硫酸氢铵粘性极强,能够吸附烟气中的大量飞灰,最终沉积于金属壁面或卡在层间,导致空预器堵塞,进而造成空预器运行阻力增加,且硫酸氢铵具有较强的腐蚀性,会带来后续设备的腐蚀问题。 Ammonium bisulfate has a boiling point of 350°C and a melting point of 140°C. It is hygroscopic, viscous, and corrosive, and it appears gaseous, liquid, and granular at different temperatures. Gaseous or granular ammonium bisulfate will flow with the flue gas, while liquid ammonium bisulfate is extremely viscous and can absorb a large amount of fly ash in the flue gas, eventually depositing on the metal wall or getting stuck between layers, resulting in blockage of the air preheater , which in turn increases the running resistance of the air preheater, and ammonium bisulfate is highly corrosive, which will cause corrosion problems for subsequent equipment.
为防止硫酸氢铵的形成对空预器造成堵塞,目前有如下研究方向:控制SO3的生成、控制氨逃逸、空预器改造和温度调控。 In order to prevent the formation of ammonium bisulfate from clogging the air preheater, there are currently the following research directions: control of SO 3 generation, control of ammonia escape, air preheater modification and temperature regulation.
温度调控是指通过对相应锅炉设备的运行温度进行控制或者实施设备改造,使硫酸氢铵能够顺利挥发,从而消除其不良影响。因此需对硫酸氢铵的挥发特性进行测试,以便确定硫酸氢铵的温度调控方法和进行温度的选择。 Temperature regulation refers to the control of the operating temperature of the corresponding boiler equipment or the implementation of equipment transformation, so that the ammonium bisulfate can be volatilized smoothly, thereby eliminating its adverse effects. Therefore, the volatility characteristics of ammonium bisulfate need to be tested in order to determine the temperature control method and temperature selection of ammonium bisulfate.
对于燃煤机组,烟气中飞灰含量较高的情况下,硫酸氢铵在146℃-207℃为液态,在较高温度下为气态,更高温度时会分解生成氨、三氧化硫和水。有学者对硫酸氢铵的分解特性进行了研究,发现硫酸氢铵的分解是一维相边界反应,其反应机理为 For coal-fired units, when the content of fly ash in the flue gas is high, ammonium bisulfate is liquid at 146°C-207°C, and is gaseous at higher temperatures. At higher temperatures, it will decompose to form ammonia, sulfur trioxide and water. Some scholars have studied the decomposition characteristics of ammonium bisulfate, and found that the decomposition of ammonium bisulfate is a one-dimensional phase boundary reaction, and the reaction mechanism is
该学者发现纯净的硫酸氢铵的分解温度在345℃以上,在490℃分解速率达到最大值,但对不同硫酸氢铵样品的挥发特性并无研究。 The scholar found that the decomposition temperature of pure ammonium bisulfate is above 345°C, and the decomposition rate reaches the maximum at 490°C, but there is no research on the volatility characteristics of different ammonium bisulfate samples.
专利号为CN104374667A的中国专利公开了一种超高真空热环境下材料挥发特性的测试装置,包括测试容器、真空抽气系统、加热控温测试平台、水冷控温收集平台和测控系统。该装置能够确定材料在超真空热环境下的挥发温度和挥发产物,但不能测试硫酸氢铵的挥发速率,因此无法为燃煤锅炉硫酸氢铵的温度调控提供理论依据和数据支持。 The Chinese patent with the patent number CN104374667A discloses a test device for the volatilization characteristics of materials in an ultra-high vacuum thermal environment, including a test container, a vacuum pumping system, a heating and temperature control test platform, a water-cooled temperature control collection platform and a measurement and control system. The device can determine the volatilization temperature and volatilization products of materials in an ultra-vacuum thermal environment, but cannot test the volatilization rate of ammonium bisulfate, so it cannot provide theoretical basis and data support for the temperature regulation of ammonium bisulfate in coal-fired boilers.
发明内容 Contents of the invention
本发明的目的在于针对现有技术之弊端,提供一种燃煤烟气中硫酸氢铵挥发特性的测试装置,为硫酸氢铵的温度调控提供可靠的理论依据和数据支持。 The purpose of the present invention is to provide a testing device for the volatility characteristics of ammonium bisulfate in coal-fired flue gas against the disadvantages of the prior art, so as to provide reliable theoretical basis and data support for the temperature regulation of ammonium bisulfate.
本发明所述问题是以下述技术方案实现的: Problem described in the present invention is realized with following technical scheme:
一种燃煤烟气中硫酸氢铵挥发特性的测试装置,构成中包括供氮系统、挥发系统和称量系统,所述挥发系统包括恒温炉、玻璃罩和坩埚,所述恒温炉的一侧通过进气管与供氮系统连接,另一侧设有出气管;所述玻璃罩置于恒温炉内;所述坩埚放置在玻璃罩内,其内部盛放被测试的硫酸氢铵样品;所述称量系统为电子天平,称量坩埚中硫酸氢铵样品的质量,所述测试装置的测试步骤如下: A test device for the volatilization characteristics of ammonium bisulfate in coal-fired flue gas, comprising a nitrogen supply system, a volatilization system and a weighing system, the volatilization system comprising a constant temperature furnace, a glass cover and a crucible, one side of the constant temperature furnace It is connected with the nitrogen supply system through the inlet pipe, and the other side is provided with an outlet pipe; the glass cover is placed in a constant temperature furnace; the crucible is placed in the glass cover, and the ammonium bisulfate sample to be tested is contained in it; Weighing system is an electronic balance, weighs the quality of ammonium bisulfate sample in the crucible, and the test procedure of described testing device is as follows:
a.将硫酸氢铵样品放入坩埚内,利用供氮系统向恒温炉内输入氮气,使玻璃罩、坩埚及硫酸氢铵样品均处于氮气氛围中; a. Put the ammonium bisulfate sample into the crucible, and use the nitrogen supply system to input nitrogen into the constant temperature furnace, so that the glass cover, the crucible and the ammonium bisulfate sample are all in a nitrogen atmosphere;
b.用恒温炉对玻璃罩内部的坩埚中所盛放的硫酸氢铵样品进行恒温加热; B. carry out constant temperature heating to the ammonium bisulfate sample held in the crucible inside glass cover with constant temperature furnace;
c.定时用电子天平称量坩埚质量并记录数据,利用下式计算设定温度下硫酸氢铵样品的挥发速率: c. Regularly weigh the mass of the crucible with an electronic balance and record the data, and use the following formula to calculate the volatilization rate of the ammonium bisulfate sample at the set temperature:
ν=Δm/Δt ν=Δm/Δt
其中,ν表示硫酸氢铵样品的挥发速率;Δt表示相邻两次称量硫酸氢铵样品质量的时间间隔;Δm表示时间间隔Δt内硫酸氢铵样品的质量变化量; Wherein, ν represents the rate of volatilization of the ammonium bisulfate sample; Δt represents the time interval between two adjacent weighings of the ammonium bisulfate sample quality; Δm represents the mass variation of the ammonium bisulfate sample in the time interval Δt;
d.以设定的步长改变恒温炉的设定温度,重复步骤a~步骤c,得到多个温度下的硫酸氢铵样品挥发速率数据; d. Change the set temperature of the constant temperature furnace with the set step length, repeat steps a to step c, and obtain the volatilization rate data of ammonium bisulfate samples at multiple temperatures;
e.根据记录的数据绘制硫酸氢铵样品的不同温度下挥发速率-时间曲线。 e. Draw the volatilization rate-time curves of the ammonium bisulfate sample at different temperatures according to the recorded data.
上述燃煤烟气中硫酸氢铵挥发特性的测试装置,构成中还包括冷凝系统和抽气系统,所述冷凝系统包括蛇形冷凝管、恒温水浴系统以及设置于恒温水浴系统中的循环水泵和孟氏洗瓶,所述蛇形冷凝管的一端接恒温炉的出气管,另一端经孟氏洗瓶与抽气系统连接;所述循环水泵的进水口和出水口分别接蛇形冷凝管外部套管的两端,蛇形冷凝管内的冷凝产物的组成及含量采用离子色谱法进行测定。 The test device for the volatile characteristics of ammonium bisulfate in the above-mentioned coal-fired flue gas also includes a condensation system and an air extraction system. The condensation system includes a serpentine condenser, a constant temperature water bath system, and a circulating water pump and One end of the serpentine condensing tube is connected to the outlet pipe of the constant temperature furnace, and the other end is connected to the air extraction system through the Monteggy rinsing bottle; the water inlet and outlet of the circulating water pump are respectively connected to the outside of the serpentine condensing tube The composition and content of the condensed product in the serpentine condensing tube at both ends of the casing are measured by ion chromatography.
上述燃煤烟气中硫酸氢铵挥发特性的测试装置,所述供氮系统包括氮气气源、流量计和电加热装置,所述氮气气源的排气口通过流量计与恒温炉的进气管连接,所述电加热装置安装在恒温炉的进气管上。 The test device for the volatilization characteristics of ammonium bisulfate in the above-mentioned coal-fired flue gas, the nitrogen supply system includes a nitrogen gas source, a flow meter and an electric heating device, the exhaust port of the nitrogen gas source passes through the flow meter and the inlet pipe of the constant temperature furnace connected, the electric heating device is installed on the inlet pipe of the constant temperature furnace.
上述燃煤烟气中硫酸氢铵挥发特性的测试装置,所述氮气气源为氮气钢瓶或制氮机。 The device for testing the volatilization characteristics of ammonium bisulfate in the above-mentioned coal-burning flue gas, the nitrogen gas source is a nitrogen cylinder or a nitrogen generator.
上述燃煤烟气中硫酸氢铵挥发特性的测试装置,所述玻璃罩的顶部或侧部设有罩门。 In the above-mentioned device for testing the volatilization characteristics of ammonium bisulfate in coal-burning flue gas, the top or side of the glass cover is provided with a cover door.
上述燃煤烟气中硫酸氢铵挥发特性的测试装置,所述称量系统采用电子天平。 The test device for the volatile characteristics of ammonium bisulfate in the above-mentioned coal-burning flue gas, the weighing system adopts an electronic balance.
上述燃煤烟气中硫酸氢铵挥发特性的测试装置,所述抽气系统采用真空泵。 The test device for the volatile characteristics of ammonium bisulfate in the above-mentioned coal-burning flue gas, the vacuum pump is used in the air extraction system.
上述燃煤烟气中硫酸氢铵挥发特性的测试装置,所述恒温炉在不同设定温度下对硫酸氢铵样品进行恒温加热,相邻两次称量硫酸氢铵样品质量的时间间隔Δt。 The above test device for the volatile characteristics of ammonium bisulfate in coal-burning flue gas, the constant temperature furnace heats the ammonium bisulfate sample at different set temperatures at a constant temperature, and the time interval Δt between two adjacent weighings of the ammonium bisulfate sample.
本发明通过监测硫酸氢铵样品随温度和挥发时间的变化情况得到样品的挥发特性,其测试结果可为燃煤锅炉硫酸氢铵的温度调控提供可靠的理论依据和数据支持,有利于解决硫酸氢铵引起的空预器堵塞和后续设备的腐蚀问题。 The invention obtains the volatilization characteristics of the sample by monitoring the change of the ammonium bisulfate sample with temperature and volatilization time, and the test results can provide reliable theoretical basis and data support for the temperature regulation of the ammonium bisulfate in the coal-fired boiler, which is beneficial to solve the problem of hydrogen sulfate Air preheater clogging and subsequent equipment corrosion caused by ammonium.
附图说明 Description of drawings
图1为本燃煤烟气中硫酸氢铵挥发特性的测试装置的结构示意图。 Fig. 1 is the structural representation of the test device for the volatility characteristics of ammonium bisulfate in the coal-fired flue gas.
图中各标号表示为:1-氮气气源;2-流量计;3-电加热装置;4-恒温炉;5-玻璃罩;6-坩埚;7-电子天平;8-蛇形冷凝管;9-循环水泵;10-孟氏洗瓶;11-真空泵;12-恒温水浴系统。 The labels in the figure are represented as: 1-nitrogen gas source; 2-flow meter; 3-electric heating device; 4-constant temperature furnace; 5-glass cover; 6-crucible; 7-electronic balance; 8-serpentine condenser; 9- circulating water pump; 10- Monteggia washing bottle; 11- vacuum pump; 12- constant temperature water bath system.
具体实施方式 detailed description
参看图1,本装置包括供氮系统、挥发系统、冷凝系统、抽气系统和称量系统。各系统的功能和结构如下: Referring to Figure 1, the device includes a nitrogen supply system, a volatilization system, a condensation system, an exhaust system and a weighing system. The functions and structures of each system are as follows:
供氮系统:用于为测试过程提供氮气气氛和一定的气体流速,包括氮气气源1(氮气钢瓶或制氮机)、流量计2和电加热装置3; Nitrogen supply system: used to provide nitrogen atmosphere and a certain gas flow rate for the test process, including nitrogen gas source 1 (nitrogen cylinder or nitrogen generator), flow meter 2 and electric heating device 3;
挥发系统:用于硫酸氢铵的加热挥发,包括恒温炉4、玻璃罩5和坩埚6。其中,恒温炉4内部温度可加热至200℃~500℃(包括其他温度范围),该恒温炉在前侧开门,并在两侧设进气和出气管路。玻璃罩5设侧开门,坩埚6耐500℃高温(包括更高温度); Volatility system: used for heating and volatilization of ammonium bisulfate, including constant temperature furnace 4, glass cover 5 and crucible 6. Wherein, the internal temperature of the constant temperature furnace 4 can be heated to 200° C. to 500° C. (including other temperature ranges). The constant temperature furnace has a door on the front side, and air inlet and outlet pipelines are arranged on both sides. The glass cover 5 is provided with a side door, and the crucible 6 is resistant to high temperatures of 500°C (including higher temperatures);
冷凝系统:用于硫酸氢铵挥发产物的冷凝,包括恒温水浴系统12、蛇形冷凝管8、循环水泵9和孟氏洗瓶10; Condensation system: used for condensation of volatile products of ammonium bisulfate, including constant temperature water bath system 12, serpentine condenser pipe 8, circulating water pump 9 and Monteshi washing bottle 10;
抽气系统:用于控制系统内部气压,防止气压过大,主要包括真空泵11; Air extraction system: used to control the internal air pressure of the system to prevent excessive air pressure, mainly including vacuum pump 11;
称量系统,用于称量硫酸氢铵在挥发过程中的质量变化,以获得硫酸氢铵的挥发速率,包括精密电子天平7,精度为0.1mg(包括更精确的电子天平),能够准确称量硫酸氢铵的质量在各种温度下随时间的变化。 The weighing system is used to weigh the mass change of ammonium bisulfate during volatilization to obtain the volatilization rate of ammonium bisulfate, including a precision electronic balance 7 with an accuracy of 0.1 mg (including a more accurate electronic balance), which can accurately weigh The mass of ammonium bisulfate varies with time at various temperatures.
硫酸氢铵挥发特性的测试方法:在氮气氛围中,用恒温炉4对玻璃罩5内的坩埚6中的硫酸氢铵样品恒温加热,定时用精密电子天平7称量坩埚6的质量并记录数据,在蛇形冷凝管8中获得硫酸氢铵挥发后的冷凝产物,用孟氏洗瓶10进行尾气的吸收,并在其后用真空泵11抽气,以防止系统内部气体压力过大。 The test method of ammonium bisulfate volatile characteristic: in nitrogen atmosphere, use constant temperature furnace 4 to the ammonium bisulfate sample in the crucible 6 in glass cover 5 constant temperature heating, regularly weigh the quality of crucible 6 with precision electronic balance 7 and record data , obtain the condensed product after ammonium bisulfate volatilizes in serpentine condensing pipe 8, carry out the absorption of tail gas with Montessori washing bottle 10, and thereafter use vacuum pump 11 to evacuate, to prevent excessive gas pressure in the system.
被测试的硫酸氢铵样品可为纯净的硫酸氢铵、不同硫酸氢铵含量的飞灰、燃煤电厂现场硫酸氢铵样品。 The ammonium bisulfate samples to be tested can be pure ammonium bisulfate, fly ash with different ammonium bisulfate content, and ammonium bisulfate samples from coal-fired power plants.
恒温炉的加热温度可在合理温度范围内选择若干个加热温度点。在每个加热温度点的测试中,每隔某个时间段,记录电子天平的示数,以获得在某测试温度下硫酸氢铵的挥发速率随时间的变化。 The heating temperature of the constant temperature furnace can choose several heating temperature points within a reasonable temperature range. During the test at each heating temperature point, record the readings of the electronic balance every certain time period to obtain the change of the volatilization rate of ammonium bisulfate with time at a certain test temperature.
硫酸氢铵挥发速率的定义为单位时间内硫酸氢铵质量的变化量,表示为: Ammonium bisulfate volatilization rate is defined as the amount of change in ammonium bisulfate quality per unit time, expressed as:
ν=Δm/Δt ν=Δm/Δt
其中,ν表示硫酸氢铵样品的挥发速率;Δt表示两次称量硫酸氢铵样品质量的时间间隔;Δm表示时间间隔Δt内硫酸氢铵样品的质量变化量。 Among them, ν represents the volatilization rate of the ammonium bisulfate sample; Δt represents the time interval between two weighings of the ammonium bisulfate sample; Δm represents the mass change of the ammonium bisulfate sample within the time interval Δt.
最后,可根据数据绘制出不同温度下挥发速率-时间曲线。 Finally, the volatilization rate-time curve at different temperatures can be drawn according to the data.
下面通过具体实施例对本发明作进一步的阐明。 The present invention will be further illustrated below by specific examples.
供氮系统选择氮气纯度>99.99%的氮气钢瓶,测量范围为0-1L/min的流量计2,电加热装置3可将气体预热至200℃。挥发系统中,恒温炉4的温度可加热至500℃,体积为50cm*50cm*20cm;玻璃罩5侧开门,其体积为20cm*20cm*10cm;陶瓷坩埚6可耐高温500℃,高度为10cm。冷凝系统中,恒温水浴系统12的温度可达100℃,用流量为2.5L/min的真空泵11抽气。称量系统选择精度为0.1mg的精密电子天平7。 The nitrogen supply system selects a nitrogen cylinder with a nitrogen purity >99.99%, a flow meter 2 with a measuring range of 0-1L/min, and an electric heating device 3 that can preheat the gas to 200°C. In the volatilization system, the temperature of the constant temperature furnace 4 can be heated to 500°C, and the volume is 50cm*50cm*20cm; the door of the glass cover 5 is opened on one side, and the volume is 20cm*20cm*10cm; the ceramic crucible 6 can withstand high temperature 500°C, and the height is 10cm . In the condensation system, the temperature of the constant temperature water bath system 12 can reach 100° C., and the vacuum pump 11 with a flow rate of 2.5 L/min is used to pump air. A precision electronic balance 7 with an accuracy of 0.1 mg was selected as the weighing system.
操作步骤为:打开氮气钢瓶,调节流量为1L/min,将电加热装置3温度调至150℃,将恒温炉4温度分别调至340℃、350℃、360℃、370℃、380℃,对某燃煤锅炉相同质量的硫酸氢铵样品进行恒温加热,在每个温度点的测试中,每隔10min用电子天平7称量坩埚6的质量并记录。在蛇形冷凝管8中观察硫酸氢铵挥发产物冷凝后的形态,对蛇形冷凝管8和孟氏洗瓶10内的凝结产物进行表征。计算挥发速率,绘制不同温度下挥发速率-时间曲线。 The operation steps are: open the nitrogen cylinder, adjust the flow rate to 1L/min, adjust the temperature of the electric heating device 3 to 150°C, and adjust the temperature of the constant temperature furnace 4 to 340°C, 350°C, 360°C, 370°C, and 380°C respectively. Ammonium bisulfate samples of the same quality in a coal-fired boiler were heated at a constant temperature. During the test at each temperature point, the mass of the crucible 6 was weighed and recorded with an electronic balance 7 every 10 minutes. In the serpentine condensing tube 8, observe the condensed form of the volatile product of ammonium bisulfate, and characterize the condensed products in the serpentine condensing tube 8 and the Monteggia washing bottle 10. Calculate the volatilization rate and draw the volatilization rate-time curve at different temperatures.
尽管上文对本发明专利的具体实施方式给予了详细描述和说明,但是应该说明的是,任何人依据本发明专利的构想对上述实施方式进行的各种等效改变和修改,均在本发明专利的保护范围之内。 Although the specific implementation of the patent of the present invention has been described and illustrated in detail above, it should be noted that any equivalent changes and modifications made to the above-mentioned implementation by anyone based on the concept of the patent of the present invention shall be included in the patent of the present invention. within the scope of protection.
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