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CN107271323B - Real-time measuring instrument for hydrate decomposition gas - Google Patents

Real-time measuring instrument for hydrate decomposition gas Download PDF

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CN107271323B
CN107271323B CN201710583724.7A CN201710583724A CN107271323B CN 107271323 B CN107271323 B CN 107271323B CN 201710583724 A CN201710583724 A CN 201710583724A CN 107271323 B CN107271323 B CN 107271323B
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gas
hydrate
core
real
decomposition
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CN107271323A (en
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张卫东
王飞
吕俊杰
赵寿强
周晨
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China University of Petroleum East China
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    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N7/00Analysing materials by measuring the pressure or volume of a gas or vapour
    • G01N7/14Analysing materials by measuring the pressure or volume of a gas or vapour by allowing the material to emit a gas or vapour, e.g. water vapour, and measuring a pressure or volume difference
    • G01N7/16Analysing materials by measuring the pressure or volume of a gas or vapour by allowing the material to emit a gas or vapour, e.g. water vapour, and measuring a pressure or volume difference by heating the material

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Abstract

The invention discloses a real-time measuring instrument for hydrate decomposition gas. The experimental device measures the gas release amount in the hydrate decomposition process in the rock core by using a drainage method. The device can control the temperature in the reactor to carry out an experiment, wherein hydrates in the rock core are decomposed, and the discharged water is measured by an electronic balance and is collected in real time by a data collector. And processing the data to draw a decomposition gas volume change curve and a decomposition gas release rate change curve with time in the process of decomposing the hydrate in the rock core. And obtaining the decomposed gas release amount after the decomposition is finished. And (4) breaking the core, releasing hydrate in the core, and measuring the total hydrate decomposition gas release amount in the core at the moment. The ratio of the value obtained by subtracting the two values to the total hydrate decomposition gas release amount is the specific gravity of the decomposition residue.

Description

一种水合物分解气体实时测量仪A real-time measuring instrument for hydrate decomposition gas

技术领域technical field

本发明涉及水合物分解监测技术领域,是一种岩心中天然气水合物控温分解过程中可实时测量分解气体积并测量分解结束含水合物岩心分解气残余量的装置。The invention relates to the technical field of hydrate decomposition monitoring, and relates to a device that can measure the volume of decomposed gas in real time during the temperature-controlled decomposition of natural gas hydrate in the core and measure the residual amount of the decomposition gas in the core containing hydrate after decomposition.

背景技术Background technique

目前,人们水合物的开采关注度正逐渐提高,了解水合物的分解状况来指导水合物的开采成为关注的焦点。中国珠江口神狐海域天然气水合物(可燃冰)于2017年5月10日点火试采,起初的开采量很大,但随着时间,开采量的衰减速度也很快,试采第一天便有3.5万立方的开采量,但试采进行31天后总产气量达到21万立方米,平均平均日产6800立方米。积极开展水合物分解情况的研究非常重要。At present, people's attention to the exploitation of hydrates is gradually increasing, and understanding the decomposition status of hydrates to guide the exploitation of hydrates has become the focus of attention. The natural gas hydrate (combustible ice) in the Shenhu waters of the Pearl River Estuary of China was ignited for trial production on May 10, 2017. The initial production volume was large, but with time, the production volume declined rapidly. The first day of trial production There are 35,000 cubic meters of mining volume, but after 31 days of trial mining, the total gas production reaches 210,000 cubic meters, with an average daily output of 6,800 cubic meters. It is very important to actively carry out research on hydrate decomposition.

在实验室中研究岩心内水合物分解状况,对于分析实际地层中水合物的分解状况有指导意义。目前对于水合物分解的动力学研究不够,现一般使用建立模型定性分析,再通过实验定量数据计算模型参数来进行研究。现对分解数据定量测量一般使用复杂的传感器组设计的仪器进行测量。这类仪器较为复杂而且昂贵,这种测量手段不适用于一般实验室的实验研究。为解决该问题,需要设计一种可利用一般实验室器材,结构简单,操作便捷,经济实惠能广泛应用于一般实验条件下的实验仪器。同时调研中发现没有对岩心中水合物分解残余量的测量方面的研究,分解残余量对于现场采收率有一定指导意义,因此设计能够测量水合物分解残余量的装置得以对该项数据进行测量分析有重要意义。The research on the decomposition of hydrate in the core in the laboratory has guiding significance for the analysis of the decomposition of hydrate in the actual formation. At present, there is not enough research on the kinetics of hydrate decomposition. At present, the establishment of a model is generally used for qualitative analysis, and then the model parameters are calculated through experimental quantitative data for research. Quantitative measurement of decomposed data is generally carried out using instruments designed with complex sensor groups. Such instruments are complex and expensive, and this measurement method is not suitable for experimental research in general laboratories. In order to solve this problem, it is necessary to design an experimental instrument that can use general laboratory equipment, has a simple structure, is convenient to operate, and is economical and can be widely used in general experimental conditions. At the same time, it is found that there is no research on the measurement of the residual amount of hydrate decomposition in the core. The residual amount of decomposition has a certain guiding significance for the on-site recovery factor. Therefore, a device that can measure the residual amount of hydrate decomposition can be designed to measure this data. Analysis is important.

发明内容SUMMARY OF THE INVENTION

本发明所要解决的问题是针对现有设施和技术的不完善,提供一种利用排水法收集测量水合物分解气量的水合物分解气体实时测量仪。The problem to be solved by the present invention is to provide a real-time measuring instrument for hydrate decomposition gas which collects and measures the amount of hydrate decomposition gas by using the drainage method, aiming at the imperfection of existing facilities and technologies.

本发明的技术方案如下:The technical scheme of the present invention is as follows:

一种实时测量分解气体积的实验方法与装置,恒压密闭空间进行水合物分解,水合物体积减小,由于分解气的产生空间内气体体积增加,且气体体积增大量远大于水合物体积分解减少量,认为空间内气体体积增大量为水合物分解气体积。在密闭性连接化学仪器中加入水制造内有气水两相且固定容积的反应-排水容器,以其气相空间部分作为反应装置近似认为内部为恒压密闭空间,可以通过阀门分隔密闭空间分隔多余水相和气相,分隔状态可打开反应装置向其中加入待测含水合物岩心。反应装置连接至排水装置上方,连通状态液柱产生压力对反应装置有抽吸作用,水合物在其中分解,气相向下驱替液相,被驱替水从容器中排出,排出水体积等于空间气体增大体积也等于水合物分解气体积。通过数据采集系统采集排出水质量的变化规律即可利用V=m/ρ计算水的体积从而得出分解气实时体积。恒温水浴箱向反应装置提供所需的恒定温度,再对靠近水相的气相部分对产出气冷凝为统一恒定温度进行排水。反应装置上方连接由阀门隔开的可以储存岩心破坏液的容器,在正常分解完成后可通过打开阀门,利用液体重力将液体注入反应装置但不改变现有装置内气体液体总体积,岩心破坏后内部残余水合物继续分解,残余气以同样方式驱替排出水测量得到分解残余气体积。An experimental method and device for measuring the volume of decomposed gas in real time. Hydrate decomposes in a closed space with constant pressure, and the volume of hydrate decreases. Due to the increase in the volume of gas in the space where decomposed gas is generated, the increase in gas volume is much greater than that of hydrate volume decomposition. Decreased amount, it is considered that the increase in the volume of gas in the space is the volume of hydrate decomposition gas. Water is added to the airtight connection chemical instrument to produce a reaction-drainage container with two phases of gas and water and a fixed volume. The gas-phase space is used as the reaction device and the interior is approximated as a constant-pressure closed space. The closed space can be separated by a valve to separate excess Water phase and gas phase, the separation state can open the reaction device and add the hydrate core to be tested. The reaction device is connected to the top of the drainage device, the pressure generated by the liquid column in the connected state has a suction effect on the reaction device, the hydrate is decomposed in it, the gas phase displaces the liquid phase downward, and the displaced water is discharged from the container, and the volume of the discharged water is equal to the space The gas increase volume is also equal to the hydrate decomposition gas volume. By collecting the variation law of the discharged water quality through the data acquisition system, the volume of water can be calculated by V=m/ρ, and the real-time volume of the decomposed gas can be obtained. The constant temperature water bath box provides the required constant temperature to the reaction device, and then the gas phase near the water phase condenses the produced gas to a uniform constant temperature for drainage. The top of the reaction device is connected to a container that can store the core-breaking liquid separated by a valve. After the normal decomposition is completed, the valve can be opened to inject the liquid into the reaction device by liquid gravity without changing the total volume of gas and liquid in the existing device. The internal residual hydrate continues to decompose, and the residual gas displaces the discharged water in the same way to measure the volume of the decomposed residual gas.

附图说明Description of drawings

图1为根据本发明水合物分解气体实时测量仪的结构示意图。FIG. 1 is a schematic structural diagram of a real-time measuring instrument for hydrate decomposition gas according to the present invention.

图中:1—恒压分液漏斗;2,3,8,14—阀门;4,7—具阀门弯接头;5—三口开口反应器;6—恒温水浴箱;9,11,15—密封的导管连接器;10—冷凝管;12—弯接头;13—梨形分液漏斗;16—排水导管;17—烧杯;18—电子天平;19—数据采集器;20—铁架台。In the figure: 1—constant pressure separatory funnel; 2,3,8,14—valve; 4,7—bend joint with valve; 5—three-port opening reactor; 6—constant temperature water bath; 9,11,15—seal 10—condensing pipe; 12—bend joint; 13—pear-shaped separatory funnel; 16—drainage conduit; 17—beaker; 18—electronic balance; 19—data collector; 20—iron stand.

具体实施方式Detailed ways

以下结合附图和具体实施例,对本发明进行详细说明。The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.

实施例1利用排水法进行水合物分解气量测量实验的原理及实施步骤Example 1 The principle and implementation steps of the measurement experiment of the hydrate decomposition gas volume using the drainage method

连接装置前所有阀门关闭。连接装置前先在恒压分液漏斗1中放入对应检测岩心的岩心破坏液并对顶端封口处理,在梨形分液漏斗13中装入足量水。三口开口反应器5由上方三口反应器盖和下方桶型容器组成,将桶型容器浸入恒温水浴箱6中来控制容器内温度,三口反应器盖向上口中竖直连接恒压分液漏斗1可使注液时岩心破坏液不接触反应器壁竖直落入反应器内,左右两侧口分别连接具阀门弯接头4、具阀门弯接头7。右侧具阀门弯接头7和冷凝管10的一端利用密封的导管连接器9连接对右侧驱替水相的气相冷却为一恒定温度。冷凝管10另一端用同样使用密封的导管连接器11连接弯接头,弯接头10接入梨型分液漏斗13上方接口中并用铁架台20对梨形分液漏斗进行固定,气相由上向下驱替液相。梨形分液漏斗13下方管口利用密封的导管连接器15连接排水导管16,排水导管16深入烧杯17,但不接触烧杯17这是防止排出水流令排水导管16抖动敲击烧杯影响天平读数,且排水导管16管口不能距烧杯17底过近,这是防止排水导管16管口过于接近烧杯10底,导管口中水流对烧杯10底的冲击会影响天平读数。烧杯放置在电子天平18上,电子天平18连接数据采集器19进行实时数据采集。连接好装置,便可进行实验。Close all valves before connecting the unit. Before connecting the device, put the core breaking liquid corresponding to the detected core in the constant pressure separatory funnel 1 and seal the top, and put enough water in the pear-shaped separatory funnel 13 . The three-port opening reactor 5 is composed of the upper three-port reactor cover and the lower barrel-shaped container. The barrel-shaped container is immersed in a constant temperature water bath 6 to control the temperature in the container. During injection, the core breaking liquid does not contact the reactor wall and falls vertically into the reactor, and the left and right sides are respectively connected with valve elbow joints 4 and valve elbow joints 7. The right valve elbow joint 7 and one end of the condenser pipe 10 are connected by a sealed conduit connector 9 to cool the gas phase of the right displacement water phase to a constant temperature. The other end of the condenser tube 10 is connected to the elbow joint with the same sealed conduit connector 11, the elbow joint 10 is connected to the upper interface of the pear-shaped separatory funnel 13, and the pear-shaped separatory funnel is fixed with the iron stand 20, and the gas phase is from top to bottom. Displace the liquid phase. The nozzle under the pear-shaped separatory funnel 13 is connected to the drain conduit 16 by the sealed conduit connector 15. The drain conduit 16 penetrates into the beaker 17, but does not touch the beaker 17. This is to prevent the draining water flow from causing the drain conduit 16 to vibrate and tap the beaker to affect the balance reading. In addition, the nozzle of the drainage conduit 16 cannot be too close to the bottom of the beaker 17, which is to prevent the nozzle of the drainage conduit 16 from being too close to the bottom of the beaker 10, and the impact of the water flow in the conduit opening on the bottom of the beaker 10 will affect the balance reading. The beaker is placed on the electronic balance 18, and the electronic balance 18 is connected to the data collector 19 for real-time data collection. Once the device is connected, the experiment is ready.

进行试验时,需先对装置进行气密性检测,打开阀门8、阀门14,这时整个装置只有梨形分液漏斗下方排水导管16一侧连通外界,这时若排水导管16内无下降的液柱证明装置连接气密性良好。检查完装置气密性,打开恒温水浴箱6对三口开口反应器5进行一段时间的预热,同时冷凝管10内开始通入冷凝液,除去温度对气体体积的影响。后打开阀门3,令排水导管16被液柱充满,继续放水直至烧杯17内液面没过排水导管16管口后关闭阀门3,这是防止实验初期排水导管16管口悬空,水流在空气中加速会对烧杯17进行冲击影响天平读数。为防止在打开三口开口反应器5放入待测岩心过程中梨形分液漏斗中水过量流失,关闭阀门3后关闭阀门8。对电子天平18进行调零,后打开三口开口反应器5将实验含水合物岩心放入。关闭三口开口反应器5后立刻打开阀门8,装置随水合物分解开始排水,电子天平18读数随之变化,同时利用数据采集器对天平读数实时记录,通过数据采集系统采集排出水质量的变化规律即可利用V=m/ρ计算水的体积从而得出分解气实时体积。待天平读数不再变化证明分解完成,记录最终读数作为分解气最大量。此时打开阀门2使恒压分液漏斗1中的岩心破坏液流入三口开口反应器5中,使岩心破坏从而残余水合物进一步分解放气。完成岩心破坏,待天平读数稳定记录天平读数作为分解气总量。分解气残余量比重=(分解气总量-分解气最大量)/分解气总量。When carrying out the test, it is necessary to test the air tightness of the device first, and open the valve 8 and valve 14. At this time, the entire device has only one side of the drain conduit 16 under the pear-shaped separatory funnel to communicate with the outside world. The liquid column proves that the device connection is airtight. After checking the air tightness of the device, open the constant temperature water bath 6 to preheat the three-port opening reactor 5 for a period of time, and at the same time, the condensate begins to pass into the condenser tube 10 to remove the influence of temperature on the gas volume. Then open the valve 3 to make the drain conduit 16 be filled with the liquid column, and continue to discharge water until the liquid level in the beaker 17 has not passed the drain conduit 16 orifice and then close the valve 3. This is to prevent the drain conduit 16 orifice from hanging in the air at the beginning of the experiment, and the water flow in the air. Acceleration will shock the beaker 17 and affect the balance reading. In order to prevent excessive loss of water in the pear-shaped separatory funnel during the process of opening the three-port opening reactor 5 and putting it into the core to be tested, close the valve 3 and then close the valve 8. The electronic balance 18 was zero-adjusted, and then the three-port opening reactor 5 was opened to put the experimental hydrate-containing core. Immediately after closing the three-port opening reactor 5, open the valve 8, the device begins to drain water with the decomposition of hydrate, and the reading of the electronic balance 18 changes accordingly. The volume of water can be calculated by V=m/ρ to obtain the real-time volume of decomposed gas. When the balance reading no longer changes to prove the decomposition is complete, record the final reading as the maximum amount of decomposition gas. At this time, the valve 2 is opened so that the core breaking liquid in the constant pressure separatory funnel 1 flows into the three-port opening reactor 5, so that the core is broken and the residual hydrate is further decomposed into gas. Complete the core destruction, and record the balance reading as the total amount of decomposed gas after the balance reading is stable. Specific gravity of residual amount of decomposed gas=(total amount of decomposed gas-maximum amount of decomposed gas)/total amount of decomposed gas.

Claims (4)

1.一种 水合物分解气体实时测量仪,主要包括:以恒压分液漏斗为主的岩心破坏装置:以三口开口反应器、恒温水浴箱、冷凝管为主的分解气反应装置;以梨形分液漏斗、烧杯为主的排水装置,以电子天平、数据采集器为主的数据收集装置,其特征在于:三口开口反应器下方浸没于恒温水浴箱,水合物分解的环境温度由水浴温度控制,三口开口反应器与梨形分液漏斗间连接冷凝管对驱替水相的气体冷却为某一恒定温度,三口开口反应器连接至梨形分液漏斗上方,气相向下驱替液相,梨形分液漏斗下方设置有烧杯,梨形分液漏斗中的液体可通过排水导管进入烧杯,烧杯放置于电子天平上,数据采集器连接电子天平并收集电子天平测量的数据,储存岩心破坏液的恒压分液漏斗连接在三口开口反应器上方,打开阀门,破坏液受重力流入反应装置和岩心接触破坏岩心,连通的恒压分液漏斗可进行恒压注液,水合物在反应装置内定温分解产气驱替排水装置中水,分解结束用岩心破坏装置破坏岩心对残余气排水,由数据收集装置完成数据采集。1. A real-time measuring instrument for hydrate decomposition gas, mainly comprising: a core destruction device based on a constant pressure separatory funnel; a decomposition gas reaction device based on a three-port opening reactor, a constant temperature water bath box, and a condensation pipe; The drainage device is mainly composed of a separatory funnel and a beaker, and the data collection device is mainly composed of an electronic balance and a data collector. It is characterized in that: the bottom of the three-port open reactor is immersed in a constant temperature water bath, and the ambient temperature of hydrate decomposition is determined by the water bath temperature. Control, a condenser tube is connected between the three-port opening reactor and the pear-shaped separatory funnel to cool the gas displacing the water phase to a certain constant temperature, and the three-port opening reactor is connected to the top of the pear-shaped separatory funnel, and the gas phase displaces the liquid phase downward. , There is a beaker under the pear-shaped separatory funnel. The liquid in the pear-shaped separatory funnel can enter the beaker through the drainage conduit. The beaker is placed on the electronic balance. The data collector is connected to the electronic balance and collects the data measured by the electronic balance. The constant pressure separatory funnel of the liquid is connected above the three-port opening reactor, and the valve is opened, and the destructive liquid flows into the reaction device by gravity and contacts the core to destroy the core. The internal temperature is decomposed to generate gas to displace the water in the drainage device. After the decomposition, the core is destroyed by the core destruction device to drain the residual gas, and the data collection device completes the data collection. 2.根据权利要求1所述的水合物分解气体实时测量仪,其特征在于:气相在排水装置中所驱替的水相的体积即为分解气体积。2 . The real-time measuring instrument for hydrate decomposition gas according to claim 1 , wherein the volume of the water phase displaced by the gas phase in the drainage device is the volume of the decomposed gas. 3 . 3.根据权利要求1所述的水合物分解气体实时测量仪,其特征在于:被驱替的水排出,收集,天平称量,利用V=m/ρ计算体积。3 . The real-time measuring instrument for hydrate decomposition gas according to claim 1 , wherein the displaced water is discharged, collected, weighed by a balance, and the volume is calculated by V=m/ρ. 4 . 4.根据权利要求1所述的水合物分解气体实时测量仪,其特征在于:天平连接数据采集器,装置连续排水,天平示数实时变化,可对天平显示数值实时记录。4. The real-time measuring instrument for hydrate decomposition gas according to claim 1, characterized in that: the balance is connected to the data collector, the device continuously drains water, and the displayed value of the balance changes in real time, and the displayed value of the balance can be recorded in real time.
CN201710583724.7A 2017-07-18 2017-07-18 Real-time measuring instrument for hydrate decomposition gas Expired - Fee Related CN107271323B (en)

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