CN203164076U - Device for determining gas-liquid chemical reaction rate based on volumetric method - Google Patents
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Abstract
一种基于容量法测定气液化学反应速率的装置,属于化学反应工程领域。由气源系统、真空系统、气体计量系统、气液反应系统、加热系统、搅拌系统、冷却系统和数据采集系统八部分组成。溶液和磁力搅拌子通过进液口置于气液反应腔中,用真空泵对计量腔和气液反应腔抽真空,去除残余气体,关闭真空电磁阀,向计量腔放入指定压力的气体,计算其摩尔数,关闭气源电磁阀,然后对溶液进行控温和搅拌,当达到反应条件时,打开均压电磁阀,向气液反应腔注入反应气体,当压力平衡时,关闭均压电磁阀,通过监测气液反应腔内气体压力随时间的变化获得化学反应的速率。本实用新型装置测试过程自动化,控温与测温精度高,操作方便。
The invention relates to a device for measuring gas-liquid chemical reaction rate based on a volumetric method, which belongs to the field of chemical reaction engineering. It consists of eight parts: gas source system, vacuum system, gas metering system, gas-liquid reaction system, heating system, stirring system, cooling system and data acquisition system. The solution and the magnetic stirrer are placed in the gas-liquid reaction chamber through the liquid inlet, and the metering chamber and the gas-liquid reaction chamber are evacuated by a vacuum pump to remove residual gas, and the vacuum solenoid valve is closed, and the gas at a specified pressure is put into the metering chamber, and its Mole number, close the gas source solenoid valve, and then control and stir the solution. When the reaction conditions are reached, open the pressure equalization solenoid valve and inject the reaction gas into the gas-liquid reaction chamber. When the pressure is balanced, close the pressure equalization solenoid valve. The rate of chemical reaction is obtained by monitoring the change of gas pressure in the gas-liquid reaction chamber with time. The utility model has the advantages of automatic testing process, high precision of temperature control and temperature measurement, and convenient operation.
Description
技术领域 technical field
本实用新型属于化学反应工程领域,涉及一种基于容量法测定气液化学反应速率的装置,适于测定气体与液体发生化学反应时的速率常数,并获得相应的速率方程。 The utility model belongs to the field of chemical reaction engineering, and relates to a device for measuring gas-liquid chemical reaction rate based on a volumetric method, which is suitable for measuring the rate constant when gas and liquid undergo chemical reactions, and obtaining a corresponding rate equation.
背景技术 Background technique
气液反应是化学反应工程中典型的过程控制环节,在工业、医疗、教学、科研等领域发挥着重要的作用。如,发电厂或窑炉尾气中采用湿法脱除SO2、合成氨工业中用铜氨溶液吸收CO、工业沼气中采用碱性溶液吸收CO2、铜洗气中采用NaOH溶液吸收残余CO2、化学分析中采用铜氨溶液标定氧浓度、医用氧中采用银氨溶液检测微量CO等。反应速率的快慢决定了原料的投放能力、产品的输出能力以及反应容器的大小,直接影响企业的一次性投资与运行维护成本,高效的反应条件对于降低能耗、提高效率和增加利润具有重要的意义,因此,测定化学反应的速率及获得相应速率方程是解决上述问题的关键。 Gas-liquid reaction is a typical process control link in chemical reaction engineering, and plays an important role in the fields of industry, medical treatment, teaching, and scientific research. For example, wet method is used to remove SO 2 from power plants or kiln tail gas, copper ammonia solution is used to absorb CO in ammonia synthesis industry, alkaline solution is used to absorb CO 2 in industrial biogas, NaOH solution is used to absorb residual CO 2 in copper scrubbing, In chemical analysis, copper ammonia solution is used to calibrate the oxygen concentration, and in medical oxygen, silver ammonia solution is used to detect trace CO, etc. The speed of reaction determines the input capacity of raw materials, the output capacity of products and the size of the reaction vessel, which directly affects the one-time investment and operation and maintenance costs of the enterprise. Efficient reaction conditions play an important role in reducing energy consumption, improving efficiency and increasing profits. Therefore, the key to solving the above problems is to measure the rate of chemical reaction and obtain the corresponding rate equation.
通常,气液反应中液体的浓度采用滴定法、色谱法或pH值法等进行人工测定,数据获取滞后,无法得到化学反应速率的瞬时值,影响了数据的测量精准度;而气体是一种可压缩介质,无论作为反应物还是生成物,其体积或压强都会随反应的进行发生瞬时变化,对化学反应过程进行紧密跟踪,反映出了化学反应的实时状况。此外,对于高温高压反应条件,取液分析过程更加困难,在常温常压下测量液体性质无法反映高温高压状态时的具体情况,而此时气体性质的变化更加灵敏,测量气体的物性参数扩大了化学反应速率的测量范围。 Usually, the concentration of the liquid in the gas-liquid reaction is manually measured by titration, chromatography or pH value method, etc., the data acquisition lags behind, and the instantaneous value of the chemical reaction rate cannot be obtained, which affects the measurement accuracy of the data; and gas is a kind of The compressible medium, whether it is a reactant or a product, its volume or pressure will change instantaneously with the progress of the reaction, and the chemical reaction process is closely tracked, reflecting the real-time status of the chemical reaction. In addition, for high-temperature and high-pressure reaction conditions, the liquid analysis process is more difficult, and the measurement of liquid properties at room temperature and pressure cannot reflect the specific conditions of high-temperature and high-pressure conditions. At this time, the change of gas properties is more sensitive, and the physical parameters of the measured gas have expanded. The measurement range for the rate of a chemical reaction.
目前,测定化学反应速率的报道多见于教学实验,如,“测量锌与硫酸反应速率实验装置的改进”一文(实验教学与仪器,2010,(9):30)采用注射器计量气体的体积“‘不同催化剂对过氧化氢分解反应速率影响’实验装置设计与探究”一文(沧州师范专科学校学报,2008,24(3):42)采用皂泡流量计测定产生气体的体积;“盐酸和醋酸反应速率对比及电离平衡移动实验装置”一文(教学仪器与实验,2004,(4):31-32)采用量筒测定产生气体的体积。这些方法属于恒压法,通过测量气体体积变化计算化学反应速率,其不足之处较为明显。首先,注射器、皂泡流量计或量筒等无法实现对体积的自动测量,必须人为操作和读取示数,增加了示值误差和主观性;其次,气体测量过程中,由于容器内残留气体、摩擦阻力或皂泡破灭造成的误差难以消除;再次,这类实验均采用玻璃容器,无法适用于高压或高温反应条件;最后,对于复杂条件反应速率测量过程,由于无法实现自动化,增加了劳动成本,难以提高效率。 At present, reports on the determination of chemical reaction rates are mostly found in teaching experiments. For example, the article "Improvement of Experimental Devices for Measuring the Reaction Rate of Zinc and Sulfuric Acid" (Experimental Teaching and Instruments, 2010, (9): 30) uses a syringe to measure the volume of gas "' The effect of different catalysts on the reaction rate of hydrogen peroxide decomposition'Experimental device design and exploration" (Journal of Cangzhou Teachers College, 2008, 24 (3): 42) uses soap bubble flowmeter to measure the volume of gas generated; "Reaction of hydrochloric acid and acetic acid The article “Experimental Device for Rate Comparison and Ionization Balance Movement” (Teaching Instruments and Experiments, 2004, (4): 31-32) uses a graduated cylinder to measure the volume of the generated gas. These methods belong to the constant pressure method, and the chemical reaction rate is calculated by measuring the gas volume change, and its shortcomings are obvious. First of all, syringes, soap bubble flowmeters or measuring cylinders cannot automatically measure the volume, and must be manually operated and read, which increases the error and subjectivity of the indication; secondly, during the gas measurement process, due to the residual gas in the container, Errors caused by frictional resistance or soap bubble collapse are difficult to eliminate; thirdly, such experiments all use glass containers, which cannot be applied to high-pressure or high-temperature reaction conditions; finally, for the reaction rate measurement process under complex conditions, the labor cost is increased due to the inability to realize automation , it is difficult to improve efficiency.
发明内容 Contents of the invention
本实用新型的目的在于开发一种基于容量法测定气液化学反应速率的装置,通过恒容变压方式在保证气体体积不变条件下通过高精度压力传感器能够对气体压强进行实时动态测量,避免了传统恒压法测量体积无法实现自动化,增加了劳动成本,难以提高效率的弊端,具有实时性和可靠性。 The purpose of this utility model is to develop a device based on the volumetric method to measure the gas-liquid chemical reaction rate. Through the constant volume variable pressure method, the gas pressure can be dynamically measured in real time through a high-precision pressure sensor under the condition that the gas volume is constant, so as to avoid It eliminates the shortcomings of the traditional constant pressure method that cannot be automated in measuring volume, increases labor costs, and is difficult to improve efficiency. It has real-time and reliability.
一种基于容量法测定气液化学反应速率的装置,是利用恒容法采用缓冲容器分步计量进气或分步计量出气的方式对反应物或生成物进行控制,通过监测化学反应中气体压强的变化适时计算反应物的消耗或生成物的产出速率,从而计算出化学反应过程的速率常数及速率方程。该装置由气源系统、真空系统、气体计量系统、气液反应系统、加热系统、搅拌系统、冷却系统和数据采集系统八部分组成。 A device for measuring the gas-liquid chemical reaction rate based on the volumetric method, which uses the constant volume method to control the reactants or products by using the buffer container to measure the gas intake or gas output step by step, and monitor the gas pressure in the chemical reaction The consumption of reactants or the output rate of products can be calculated in due course, so as to calculate the rate constant and rate equation of the chemical reaction process. The device consists of eight parts: gas source system, vacuum system, gas metering system, gas-liquid reaction system, heating system, stirring system, cooling system and data acquisition system.
其中所述气源系统由待测气源气瓶、减压阀、气源电磁阀和气源连接法兰组成。待测气源气瓶用于盛放参加化学反应的气体,由于气瓶压力较高,需要经过减压阀将压力减至化学反应操作所需压力,减压阀通过高压密封螺纹与待测气源气瓶相连。气源电磁阀由程序控制打开或关闭,用于控制经过减压的待测气源进入计量腔,气源电磁阀通过管路与减压阀和气源连接法兰相连,气源连接法兰用于连接气源系统和计量腔。 The gas source system is composed of a gas source cylinder to be tested, a pressure reducing valve, a gas source solenoid valve and a gas source connection flange. The gas source gas cylinder to be tested is used to hold the gas that participates in the chemical reaction. Due to the high pressure of the gas cylinder, the pressure needs to be reduced to the pressure required for the chemical reaction operation through the pressure reducing valve. The pressure reducing valve is connected with the gas to be tested through the high pressure sealing thread connected to the source gas cylinder. The air source solenoid valve is opened or closed by program control, and is used to control the decompressed air source to be measured to enter the metering chamber. The air source solenoid valve is connected with the pressure reducing valve and the air source connecting flange through the pipeline, and the air source connecting flange For connecting the air supply system and the metering chamber.
所述真空系统由真空连接法兰、真空电磁阀和真空泵组成。真空系统通过真空连接法兰与计量腔相接,用于对计量腔抽真空,排除残余气体的影响。真空泵、真空电磁阀和真空连接法兰通过管路相连,真空电磁阀由程序控制打开或关闭。 The vacuum system consists of a vacuum connecting flange, a vacuum solenoid valve and a vacuum pump. The vacuum system is connected with the metering chamber through the vacuum connection flange, which is used to evacuate the metering chamber and eliminate the influence of residual gas. The vacuum pump, the vacuum solenoid valve and the vacuum connection flange are connected through pipelines, and the vacuum solenoid valve is opened or closed by program control.
所述气体计量系统由计量腔、计量腔热电偶套管、计量腔热电偶、均压连接法兰、计量腔测压连接法兰和计量腔压力传感器组成。计量腔热电偶置于计量腔热电偶套管内,计量腔热电偶套管伸入计量腔内,通过焊接工艺与计量腔连接在一起,计量腔热电偶用于测定计量腔内气体的温度。计量腔压力传感器通过计量腔测压连接法兰与计量腔相连,用于测定计量腔内气体的压力。计量腔通过均压连接法兰与均压电磁阀相连。 The gas metering system is composed of a metering chamber, a metering chamber thermocouple casing, a metering chamber thermocouple, a pressure equalizing connection flange, a metering chamber pressure measuring connection flange and a metering chamber pressure sensor. The thermocouple of the metering chamber is placed in the thermocouple casing of the metering chamber, and the thermocouple casing of the metering chamber extends into the metering chamber, and is connected with the metering chamber through a welding process. The thermocouple of the metering chamber is used to measure the temperature of the gas in the metering chamber. The metering chamber pressure sensor is connected with the metering chamber through the metering chamber pressure measuring connecting flange, and is used to measure the pressure of the gas in the metering chamber. The metering chamber is connected with the pressure equalizing solenoid valve through the pressure equalizing connecting flange.
所述气液反应系统由均压电磁阀、反应腔压力传感器、气液反应腔、进液口、气体测温偶套管、气体测温热电偶、液体测温偶套管和液体测温热电偶组成;气体测温热电偶置于气体测温偶套管内,气体测温偶套管插入气液反应腔上部,通过焊接工艺与气液反应腔连接在一起,气体测温热电偶用于测定气液反应腔上部空间气体的温度;液体测温热电偶置于液体测温偶套管内,液体测温偶套管插入气液反应腔下部,但高于磁力搅拌子高度,通过焊接工艺与气液反应腔连接在一起,液体测温热电偶用于测定气液反应腔下部空间液体的温度;进液口为带有方形螺母的管路,与气液反应腔通过焊接工艺连接在一起,用于放入或倒出液体,放入或倒出磁力搅拌子,工作时,通过配套螺栓密封;反应腔压力传感器通过螺纹安装在Y形冷却蛇管上方,用于测定气液反应腔内气体的压力,当气液反应温度较高时,通过冷却水套内的冷却介质将液体蒸汽冷却,保证反应腔压力传感器测得的是反应气体的压力;Y形冷却蛇管内径介于4~7mm,内径过大,热传导冷却效果差,内径过小,冷凝的液体由于表面张力会堵塞管路; The gas-liquid reaction system consists of a pressure equalizing solenoid valve, a reaction chamber pressure sensor, a gas-liquid reaction chamber, a liquid inlet, a gas thermocouple casing, a gas temperature-measuring thermocouple, a liquid thermocouple casing and a liquid temperature-measuring thermoelectric Couple composition; the gas temperature measuring thermocouple is placed in the gas thermocouple casing, the gas temperature measuring casing is inserted into the upper part of the gas-liquid reaction chamber, and connected with the gas-liquid reaction chamber through welding process, and the gas temperature measuring thermocouple is used to measure The temperature of the gas in the upper space of the gas-liquid reaction chamber; the liquid thermocouple is placed in the liquid thermocouple sleeve, and the liquid thermocouple sleeve is inserted into the lower part of the gas-liquid reaction chamber, but it is higher than the height of the magnetic stirrer. Through the welding process and the gas The liquid reaction chambers are connected together, and the liquid temperature measuring thermocouple is used to measure the temperature of the liquid in the lower space of the gas-liquid reaction chamber; the liquid inlet is a pipeline with a square nut, which is connected with the gas-liquid reaction chamber through a welding process. When putting in or pouring out the liquid, putting in or pouring out the magnetic stirrer, it is sealed by matching bolts when working; the pressure sensor of the reaction chamber is installed above the Y-shaped cooling coil through threads, and is used to measure the pressure of the gas in the gas-liquid reaction chamber , when the gas-liquid reaction temperature is high, the liquid vapor is cooled by the cooling medium in the cooling water jacket to ensure that the reaction chamber pressure sensor measures the pressure of the reaction gas; the inner diameter of the Y-shaped cooling coil is between 4 and 7mm, and Large, the heat conduction cooling effect is poor, the inner diameter is too small, the condensed liquid will block the pipeline due to surface tension;
所述气体加热系统由加热丝、金属均热片、控温热电偶、加热线缆和控温仪表组成。加热丝通过绝缘材料均匀缠绕在金属均热片内部,通过加热线缆与控温仪表相连,控温热电偶置于金属均热片内部,与气液反应腔紧密接触,达到快速测温和控温的作用。金属均热片环绕在气液反应腔外围,其底端通过金属压边工艺吻合在一起,金属均热片将加热丝产生的热量均匀分布在气液反应腔的外壁,通过热传导方式对气液反应腔内部反应物进行加热。 The gas heating system is composed of a heating wire, a metal spreader, a temperature control thermocouple, a heating cable and a temperature control instrument. The heating wire is evenly wound inside the metal heat spreader through the insulating material, and connected to the temperature control instrument through the heating cable. The temperature control thermocouple is placed inside the metal heat spreader and is in close contact with the gas-liquid reaction chamber to achieve rapid temperature measurement and control. The role of temperature. The metal heat spreader surrounds the periphery of the gas-liquid reaction chamber, and its bottom ends are anastomosed together by the metal crimping process. The metal heat spreader evenly distributes the heat generated by the heating wire on the outer wall of the gas-liquid reaction chamber, and heats the gas-liquid through heat conduction. The reactants inside the reaction chamber are heated.
所述气体搅拌系统由磁力搅拌子、磁力搅拌器和搅拌加速旋钮组成。磁力搅拌子通过进液口放入气液反应腔,磁力搅拌子是由耐磨有机材料包覆的磁性材料,在旋转的运动磁场中进行圆周运动。磁力搅拌器产生旋转的磁场,通过调节搅拌加速旋钮可以改变旋转磁场的频率,从而改变磁力搅拌子的圆周运动速度。 The gas stirring system consists of a magnetic stirrer, a magnetic stirrer and a stirring acceleration knob. The magnetic stirrer is put into the gas-liquid reaction chamber through the liquid inlet. The magnetic stirrer is a magnetic material coated with wear-resistant organic materials, and it performs circular motion in the rotating moving magnetic field. The magnetic stirrer generates a rotating magnetic field, and the frequency of the rotating magnetic field can be changed by adjusting the stirring acceleration knob, thereby changing the circular motion speed of the magnetic stirrer.
所述冷却系统由冷却水套、冷却水套入口、冷却水套出口、Y形冷却蛇管和蛇管连接法兰组成。Y形冷却蛇管上部为Y形分叉,使冷凝液体流入气液反应腔,下部为盘旋上升的蛇管或螺旋形管路,最下端通过蛇管连接法兰与气液反应腔相连。Y形冷却蛇管外部流过冷却介质,冷却介质从冷却水套入口进入,从冷却水套出口溢出。Y形冷却蛇管与冷却水套(16)通过焊接连接在一起。 The cooling system is composed of a cooling water jacket, an inlet of the cooling water jacket, an outlet of the cooling water jacket, a Y-shaped cooling coil and a connecting flange of the coil. The upper part of the Y-shaped cooling coil is a Y-shaped bifurcation, which allows the condensed liquid to flow into the gas-liquid reaction chamber. The lower part is a coiled or spiral pipeline that spirals upward. The bottom end is connected to the gas-liquid reaction chamber through a coil connecting flange. The cooling medium flows through the outside of the Y-shaped cooling coil, and the cooling medium enters from the inlet of the cooling water jacket and overflows from the outlet of the cooling water jacket. The Y-shaped cooling coil and the cooling water jacket (16) are connected together by welding.
所述数据采集系统由数据采集与阀门控制电路板和上位计算机组成。数据采集与阀门控制电路板将计量腔热电偶、气体测温热电偶、液体测温热电偶、计量腔压力传感器和反应腔压力传感器传入的电压或电流模拟信号转化为数字信号后传入上位计算机作为计算数据。当压力条件满足设定要求时,上位计算机向数据采集与阀门控制电路板发送数字开关指令,数据采集与阀门控制电路板将数字信号转化为电压信号,驱动气源电磁阀、真空电磁阀或均压电磁阀打开或闭合,实现程序的自动控制。 The data acquisition system is composed of a data acquisition and valve control circuit board and a host computer. The data acquisition and valve control circuit board converts the voltage or current analog signals from the metering chamber thermocouple, gas temperature measuring thermocouple, liquid temperature measuring thermocouple, metering chamber pressure sensor and reaction chamber pressure sensor into digital signals and then transmits them to the host Computers as computational data. When the pressure conditions meet the set requirements, the host computer sends a digital switch instruction to the data acquisition and valve control circuit board, and the data acquisition and valve control circuit board converts the digital signal into a voltage signal to drive the air source solenoid valve, vacuum solenoid valve or equalizer. The pressure solenoid valve is opened or closed to realize the automatic control of the program.
所述计量腔热电偶套管、气体测温偶套管和液体测温偶套管前端经过加工减薄,增强热传导性能,其壁厚不超过0.3 mm,从而提高计量腔热电偶、气体测温热电偶和测体测温热电偶的灵敏度。 The thermocouple casing of the metering chamber, the gas thermocouple casing and the liquid thermocouple casing are processed and thinned at the front end to enhance the heat conduction performance. Sensitivity of thermocouples and body temperature thermocouples.
所述的基于容量法测定气液化学反应速率的装置的气液反应速率测试过程如下:首先,将磁力搅拌子通过进液口置于气液反应腔内,将配制好的溶液通过漏斗经进液口放入气液反应腔内,密封进液口,将气液反应腔置于磁力搅拌器上,打开磁力搅拌器开关,旋转搅拌加速旋钮,使磁力搅拌子在液体中进行旋转运动,打开控温仪表,设定加热温度,对气液反应腔进行温度控制,打开上位计算机和数据采集与阀门控制电路板。然后,打开真空泵,打开真空电磁阀、均压电磁阀和气源电磁阀,对气路和腔体进行抽真空,去除杂质气体和液体上部蒸汽,当压力达到指定值时,关闭真空电磁阀、气源电磁阀和均压电磁阀,打开待测气源气瓶,当减压阀压力调整到指定压力值时,打开气源电磁阀,当计量腔压力传感器所测压力值和计量腔热电偶所测温度稳定后,记录计量腔内气体压力值和温度值,由于计量腔体积为已知,根据气体状态方程计算进入计量腔的气体摩尔数。之后,待气液反应腔中的液体测温热电偶数值与控温仪表设定值相差恒定时,记录反应腔压力传感器的压力值和气体测温热电偶的温度值,根据气液反应腔体积和所装溶液体积计算气液反应腔上部空间气体体积,再根据气体状态方程计算液体蒸汽的摩尔数。此时,打开均压电磁阀,由于计量腔内气体压力高于气液反应腔内蒸汽压力,计量腔内的气体经均压电磁阀进入气液反应腔,与液体发生化学反应,当计量腔压力传感器所测压力数值与反应腔压力传感器所测压力值差值恒定时,关闭均压电磁阀,通过数据采集与阀门控制电路板记录气液反应腔内压力随时间的变化值,根据道尔顿分压定律可以计算出气液反应腔内气体减少的摩尔数,从而计算出气液反应的速率。 The test process of the gas-liquid reaction rate of the device for measuring the gas-liquid chemical reaction rate based on the volumetric method is as follows: first, a magnetic stirrer is placed in the gas-liquid reaction chamber through the liquid inlet, and the prepared solution is passed through the funnel through the inlet. Put the liquid port into the gas-liquid reaction chamber, seal the liquid inlet, place the gas-liquid reaction chamber on the magnetic stirrer, turn on the switch of the magnetic stirrer, turn the stirring acceleration knob to make the magnetic stirrer rotate in the liquid, open The temperature control instrument sets the heating temperature, controls the temperature of the gas-liquid reaction chamber, and turns on the upper computer and the data acquisition and valve control circuit board. Then, turn on the vacuum pump, open the vacuum solenoid valve, pressure equalization solenoid valve and air source solenoid valve, vacuumize the gas circuit and cavity, remove impurity gas and liquid upper vapor, and when the pressure reaches the specified value, close the vacuum solenoid valve, Air source solenoid valve and pressure equalization solenoid valve, open the gas source cylinder to be measured, when the pressure of the pressure reducing valve is adjusted to the specified pressure value, open the air source solenoid valve, when the pressure value measured by the pressure sensor of the metering chamber and the thermocouple of the metering chamber After the measured temperature is stable, record the gas pressure and temperature values in the metering chamber. Since the volume of the metering chamber is known, the number of moles of gas entering the metering chamber is calculated according to the gas state equation. Afterwards, when the difference between the value of the liquid temperature measuring thermocouple in the gas-liquid reaction chamber and the set value of the temperature control instrument is constant, record the pressure value of the pressure sensor in the reaction chamber and the temperature value of the gas temperature measuring thermocouple, according to the volume of the gas-liquid reaction chamber Calculate the gas volume in the upper space of the gas-liquid reaction chamber with the volume of the solution contained, and then calculate the moles of liquid vapor according to the gas state equation. At this time, open the pressure equalizing solenoid valve, because the gas pressure in the metering chamber is higher than the vapor pressure in the gas-liquid reaction chamber, the gas in the metering chamber enters the gas-liquid reaction chamber through the pressure equalizing solenoid valve, and chemically reacts with the liquid. When the difference between the pressure value measured by the pressure sensor and the pressure value measured by the pressure sensor in the reaction chamber is constant, the pressure equalizing solenoid valve is closed, and the pressure in the gas-liquid reaction chamber changes with time through the data acquisition and valve control circuit board. The law of partial pressure can calculate the number of moles of gas reduced in the gas-liquid reaction chamber, thereby calculating the rate of the gas-liquid reaction.
所述的Y形冷却蛇管的长度和冷却水套内冷却介质的温度由实际需要确定,保证反应腔压力传感器处无冷凝液体。 The length of the Y-shaped cooling coil and the temperature of the cooling medium in the cooling water jacket are determined according to actual needs to ensure that there is no condensed liquid at the pressure sensor in the reaction chamber.
所述的控温热电偶可以采用符合控温精度要求的热电阻、热敏电阻等测温元器件。 The temperature-controlling thermocouple can adopt temperature-measuring components such as thermal resistors and thermistors that meet the temperature-controlling accuracy requirements.
所述的金属均热片采用导热性能良好的紫铜、铝或不锈钢等材质。 The metal heat spreader is made of copper, aluminum or stainless steel with good thermal conductivity.
所述的计量腔热电偶、液体测温热电偶和气体测温热电偶可以分别采用符合现场精度要求的其它测温元器件,如热电阻、热敏电阻等替代。 The metering chamber thermocouple, liquid temperature measuring thermocouple and gas temperature measuring thermocouple can be replaced by other temperature measuring components that meet the field accuracy requirements, such as thermal resistors and thermistors.
本实用新型提出的计量腔恒容测压、气液分离测温、环形金属均匀加热、外置加热控温、冷却除液、分剂量投放反应气等方式保证了该发明装置测试性能的稳定可靠,简单方便,是研究气液反应速率有力的试验装置,适用于不同温度、不同压力下各种气体与液体的反应,根据需要还可以测定液体解吸气体逆过程的反应速率以及气液反应处于动态平衡时的静态气体吸收量。 The utility model proposes methods such as constant volume pressure measurement of the metering chamber, gas-liquid separation temperature measurement, uniform heating of the annular metal, external heating temperature control, cooling and liquid removal, and divided dosage of reaction gas to ensure the stability and reliability of the test performance of the device of the invention. , simple and convenient, it is a powerful test device for studying the gas-liquid reaction rate, suitable for the reaction of various gases and liquids at different temperatures and pressures, and can also measure the reaction rate of the liquid desorption gas reverse process and the dynamic state of the gas-liquid reaction Static gas uptake at equilibrium.
附图说明 Description of drawings
图1是本实用新型装置的工作原理示意图; Fig. 1 is the working principle schematic diagram of the utility model device;
图1中:1. 待测气源气瓶;2. 减压阀;3. 气源电磁阀;4. 气源连接法兰;5. 计量腔;6. 计量腔热电偶套管;7. 计量腔热电偶;8. 均压连接法兰;9. 计量腔测压连接法兰;10. 计量腔压力传感器;11. 真空连接法兰;12. 真空电磁阀;13. 真空泵;14. 均压电磁阀;15. 反应腔压力传感器;16. 冷却水套;17. 冷却水套入口;18. 冷却水套出口;19. Y形冷却蛇管;20. 蛇管连接法兰;21. 气液反应腔;22. 进液口;23. 气体测温偶套管;24. 气体测温热电偶;25. 液体测温偶套管;26. 液体测温热电偶;27. 加热丝;28. 金属均热片;29. 磁力搅拌子;30. 磁力搅拌器;31. 搅拌加速旋钮;32. 控温热电偶;33. 加热线缆;34. 控温仪表;35. 数据采集与阀门控制电路板;36. 上位计算机;
In Figure 1: 1. gas cylinder to be tested; 2. pressure reducing valve; 3. gas source solenoid valve; 4. gas source connecting flange; 5. metering chamber; 6. metering chamber thermocouple sleeve; 7. Metering chamber thermocouple; 8. Pressure equalizing connecting flange; 9. Measuring chamber pressure measuring connecting flange; 10. Measuring chamber pressure sensor; 11. Vacuum connecting flange; 12. Vacuum solenoid valve; 13. Vacuum pump; 14. Average 15. Reaction chamber pressure sensor; 16. Cooling water jacket; 17. Cooling water jacket inlet; 18. Cooling water jacket outlet; 19. Y-shaped cooling coil; 20. Coil connecting flange; 21. Gas-
图2是本实用新型装置中置于容器内的所有热电偶及其套管简图; Fig. 2 is all thermocouples and sleeve pipe sketches thereof that are placed in the container in the utility model device;
6. 计量腔热电偶套管;7. 计量腔热电偶;23. 气体测温偶套管;24. 气体测温热电偶;25. 液体测温偶套管;26. 液体测温热电偶。 6. Measuring chamber thermocouple casing; 7. Measuring chamber thermocouple; 23. Gas thermocouple casing; 24. Gas temperature measuring thermocouple; 25. Liquid thermocouple casing; 26. Liquid temperature measuring thermocouple.
具体实施方式 Detailed ways
实施例测定一乙醇胺溶液(MEA)与二氧化碳气体的化学反应速率,选用30% MEA溶液500mL,计量腔5体积为500mL,气液反应腔21体积为1000mL,计量腔热电偶7、气体测温热电偶24和液体测温热电偶26均采用一级T型热电偶,其精度为±0.5℃。计量腔压力传感器10采用压力范围为0~1MPa,精度为±0.06%的压电式传感器,反应腔压力传感器15采用工作压力范围为0~0.2MPa,最大承受压力1MPa,精度为±0.06%的压阻式传感器。真空泵13抽气速率为0.5L/s,待测气源气瓶1为40L的二氧化碳气瓶,最高压力为15MPa,减压阀2最大量程为1.4MPa。冷却水套16与循环冷却水相连,循环冷却水温度控制在1±0.1℃。计量腔5的温度为室温28℃,控温仪表34温度设为40℃。
Embodiments Measure the chemical reaction rate of monoethanolamine solution (MEA) and carbon dioxide gas, select 500mL of 30% MEA solution for use, the volume of
参见图1和图2,将磁力搅拌子29和30%MEA溶液通过进液口22置于气液反应腔21内,密封进液口,将气液反应腔21置于磁力搅拌器30上,调整搅拌加速旋钮31,使磁力搅拌子29在液体中均匀旋转,打开控温仪表34,设定加热温度为40℃,打开上位计算机36和数据采集与阀门控制电路板35,打开真空泵13,打开真空电磁阀12和均压电磁阀14,对气路和腔体抽真空,当压力瞬时值低于1Pa时,关闭均压电磁阀14和真空电磁阀12,打开待测气源气瓶1,打开减压阀2,调整至1MPa。打开气源电磁阀3,向计量腔5充入1.0MPa的二氧化碳,待计量腔压力传感器10压力变化稳定后,关闭气源电磁阀3,根据气体状态方程计算计量腔5内充入二氧化碳气体的摩尔数。待气液反应腔21内液体测温热电偶26测得的温度达到40±0.1℃时,开启均压电磁阀14,当计量腔压力传感器10压力值与反应腔压力传感器15所测压力值相差满足程序设定要求时,关闭均压电磁阀14。此时,监测反应腔压力传感器15压力的变化值,对时间作曲线,直到其压力值变化率小于120Pa/s时,反应结束。根据气体测温热电偶24测得的温度40℃计算液体的蒸汽压,再根据气体状态方程和道尔顿分压定律计算进入气液反应腔21的二氧化碳摩尔量。通过反应压力曲线计算二氧化碳气体分压随时间的变化率,再通过气液反应腔21的体积计算得出化学反应速率,从而给出二氧化碳与30%MEA溶液反应的速率方程。
1 and 2, place the
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