WO2019080348A1 - 一种气体水合物晶体培养装置 - Google Patents

一种气体水合物晶体培养装置

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Publication number
WO2019080348A1
WO2019080348A1 PCT/CN2017/118899 CN2017118899W WO2019080348A1 WO 2019080348 A1 WO2019080348 A1 WO 2019080348A1 CN 2017118899 W CN2017118899 W CN 2017118899W WO 2019080348 A1 WO2019080348 A1 WO 2019080348A1
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WIPO (PCT)
Prior art keywords
high pressure
pressure resistant
culture dish
crystal culture
buffer tank
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PCT/CN2017/118899
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English (en)
French (fr)
Inventor
周雪冰
梁德青
龙臻
申小冬
Original Assignee
中国科学院广州能源研究所
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Application filed by 中国科学院广州能源研究所 filed Critical 中国科学院广州能源研究所
Priority to US16/336,911 priority Critical patent/US11046904B2/en
Publication of WO2019080348A1 publication Critical patent/WO2019080348A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
    • C30B7/10—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by application of pressure, e.g. hydrothermal processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006—Controlling or regulating processes
    • B01J19/0013—Controlling the temperature of the process
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
    • B01J19/121—Coherent waves, e.g. laser beams
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/06—Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies
    • B01J3/062—Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies characterised by the composition of the materials to be processed
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
    • B01J2219/00094—Jackets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00162—Controlling or regulating processes controlling the pressure
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
    • C10L3/00—Gaseous fuels; Natural gas; Synthetic natural gas obtained by processes not covered by subclass C10G, C10K; Liquefied petroleum gas
    • C10L3/06—Natural gas; Synthetic natural gas obtained by processes not covered by C10G, C10K3/02 or C10K3/04
    • C10L3/10—Working-up natural gas or synthetic natural gas
    • C10L3/108—Production of gas hydrates

Definitions

  • the present invention relates to the field of crystal culture equipment, and in particular to a gas hydrate crystal culture apparatus.
  • a gas hydrate is an ice-like crystalline compound having a cage structure formed of a gas molecule and a water molecule and formed under low temperature and high pressure conditions.
  • Naturally formed gas hydrates are widely distributed in deep sea sediments or continental permafrost layers.
  • the proven natural gas hydrate reserves in the world reach 2.1 ⁇ 10 16 m 3 , which is more than twice the total amount of traditional fossil energy.
  • gas hydrates have a high gas storage density.
  • a standard volume of gas hydrate can store up to 160 standard volumes of gas.
  • the temperature and pressure conditions required for storage are milder than that of liquefied gas, so it can be widely used for natural gas storage and transportation and carbon dioxide fixation and storage. Therefore, studying the kinetics and related mechanisms of gas hydrates is of great significance for realizing the exploitation, storage and transportation of natural gas hydrates and the capture and storage of greenhouse gases.
  • Gas hydrates are unstable under normal temperature and pressure conditions and are easily decomposed into gas and liquid water. Maintaining a stable hydrate crystal structure requires lower temperatures and higher pressures. For example, at 1 ° C, the minimum pressure required to maintain methane gas hydrate crystals is about 2.9 MPa. Therefore, it is difficult to perform measurement in terms of hydrate-related physical properties and crystal characteristics under ordinary conditions of room temperature and one atmosphere. At the same time, the porous nature of the gas hydrate, the non-stoichiometric properties, and the sensitivity of the crystal structure to gas pressure cause the single gas hydrate crystal to be difficult to grow into a measurable size visible to the naked eye, resulting in a single crystal on the gas hydrate. Measurements are more difficult, and studies on the growth kinetics of hydrate crystals in solution cannot be carried out. In order to complete the research and breakthrough of gas hydrate in the field of crystallography, the original equipment must be improved.
  • the invention provides a gas hydrate crystal culture device, in order to achieve the purpose of versatility, so that the measurement has more precise technical effects.
  • a gas hydrate crystal culture device comprising a mobile gantry, a temperature control system, a pressure control system, a data acquisition system and a high pressure resistant crystal culture dish, the high pressure resistant crystal culture dish, the temperature control system, the pressure control
  • the system and the data acquisition system are both mounted on the mobile gantry;
  • the high pressure resistant crystal culture dish comprises a high pressure resistant crystal culture dish body, the upper end of the high pressure resistant crystal culture dish body is provided with an incident laser window end cover, the lower end is provided with a high pressure resistant crystal culture dish fixing bracket, and the interior is provided with high pressure resistant a cavity, an incident laser window glass is disposed under the end cover of the incident laser window, and the two sides of the incident laser window glass are respectively the high pressure cavity inlet and the exhaust port, and the inlet port is connected and lengthened.
  • a gas pipe, a coolant jacket is disposed outside the high pressure chamber, and an inlet and an outlet of the coolant are located at a center of a bottom portion of the coolant jacket, and the bottom of the sidewall of the high pressure chamber is provided with the stage.
  • the high pressure cavity body is symmetrically distributed with the high pressure resistant cavity window glass, and the high pressure resistant cavity window glass is provided with a high pressure resistant cavity window end cover;
  • the temperature control system includes a cryostat and a coolant hose, and the cryostat is connected to the high pressure resistant crystal culture dish through the coolant hose, and the upper end of the high pressure resistant crystal culture dish is resistant High-pressure crystal culture dish thermocouple thermometer and high pressure crystal culture dish pressure sensor;
  • the pressure control system includes a high pressure hose, a vacuum pump needle valve, an intake buffer tank, an exhaust buffer tank, and a vacuum pump, and the high pressure resistant crystal petri dish is respectively connected to the intake buffer tank and the
  • the exhaust buffer tanks are connected to each other, and the high-pressure hoses are respectively provided with an inlet needle valve and an exhaust port needle valve, and a bypass needle valve is arranged between the intake buffer tank and the exhaust buffer tank
  • the vacuum pump is in communication with the vent needle through the vacuum pump needle valve, and the intake buffer tank is provided with an intake buffer tank pressure sensor and an intake buffer tank thermocouple thermometer, and the exhaust buffer tank An exhaust buffer thermocouple thermometer and an exhaust buffer tank pressure sensor are provided;
  • the data acquisition system includes a thermocouple thermometer and a pressure sensor, and the mobile gantry is provided with a paperless recorder, and the thermocouple thermometer and the pressure sensor transmit data to the paperless recorder.
  • the precision positioning platform is disposed in front of the high pressure resistant crystal culture dish, and the precision positioning platform is provided with a camera.
  • the mobile gantry adopts an aluminum alloy skeleton, and the rest are made of a stainless steel plate material.
  • the high pressure resistant crystal culture dish fixing bracket is a hollow structure
  • the low temperature thermostatic bath is connected to the high pressure resistant crystal culture dish through a hollow structure of the high pressure crystal culture dish fixing bracket through the coolant hose. through.
  • the stage is a detachable component; the stage is made of brass and has a "work" shape; the upper end surface of the stage is covered with a layer of polytetrafluoroethylene material; The bottom of the stage is fitted with the bottom wall of the high pressure resistant cavity and is provided with a cylindrical positioning pin.
  • the extended intake pipe is a detachable component; and the extended intake pipe is made of a stainless steel material.
  • the two side glasses on the moving gantry opposite to the high pressure resistant crystal culture dish adopt electromagnetic liquid crystal dimming glass.
  • the high-pressure resistant crystal petri dish and the internal high-pressure resistant cavity inside thereof have a flat cylindrical shape.
  • the utility model has the beneficial effects that the invention combines the experimental means of the current hydrate crystallography research, and can complete various experimental research methods such as a bubbling method, a droplet method and a solution growth method by changing the experimental accessories in the high pressure resistant crystal culture dish. Improve the versatility of the device.
  • the present invention is directed to the case where the conventional gas hydrate crystal culture device encounters low observation precision and low pressure resistance of the device, and enhances the isolation effect of the hydrate crystal culture dish enclosure structure on heat conduction and heat radiation in the external environment.
  • the incident quality and the incident mode of the background light source inside the hydrate crystal culture dish are improved, and the two-dimensional remote movement of the camera lens is realized, and the pressure resistance and low temperature resistance of the hydrate crystal culture dish are improved. This makes hydrate crystallographic measurements more precise and is used in a wider variety of hydrate crystal measurements.
  • Figure 1 is a flow chart of the operation of the present invention
  • Figure 2 is a schematic view of the structure of the present invention.
  • Figure 3 is a cross-sectional view of Figure 2 taken along line A-A';
  • Figure 4 is a schematic view showing the external structure of a high pressure resistant crystal culture dish
  • Figure 5 is a schematic view showing the internal structure of a high pressure resistant crystal culture dish
  • Figure 6 is a schematic view showing the structure of a high pressure resistant cavity
  • a gas hydrate crystal culture device comprises a mobile gantry 1, a temperature control system, a pressure control system, a data acquisition system and a high pressure resistant crystal culture dish 5, the high pressure resistant crystal culture dish 5, the temperature control system, and the The pressure control system and the data acquisition system are both mounted on the mobile gantry 1;
  • the high pressure resistant crystal culture dish 5 includes a high pressure resistant crystal culture dish body 5d.
  • the upper end of the high pressure resistant crystal culture dish body 5d is provided with an incident laser window end cover 5a, and the lower end is provided with a high pressure resistant crystal culture dish fixing bracket 5b.
  • a high-pressure resistant cavity 5x is disposed inside, and an incident laser window glass 5c is disposed under the incident laser window end cover 5a, and the two sides of the incident laser window glass 5c are respectively the high-pressure resistant cavity 5x inlet and the exhaust
  • the inlet port is connected to the elongated intake pipe, and the outer side of the high pressure resistant cavity 5x is provided with a coolant jacket 5y.
  • the inlet and the outlet of the coolant are located at the center of the bottom of the coolant jacket 5y, and the high pressure resistant cavity 5x
  • the bottom of the side wall is provided with the stage, the high-pressure resistant cavity 5x is symmetrically distributed with the high-pressure-resistant cavity window glass 5f, and the high-pressure resistant window glass 5f is provided with a high-pressure resistant window window end cover 5e. ;
  • the temperature control system includes a cryostat 3 and a coolant hose 6, and the cryostat 3 communicates with the high pressure resistant crystal culture vessel 5 through the coolant hose 6, the high pressure crystal culture
  • the upper end of the dish 5 is provided with a high pressure resistant crystal culture dish thermocouple thermometer 7 and a high pressure resistant crystal culture dish pressure sensor 12;
  • the pressure control system includes a high pressure hose 9, a vacuum pump needle 15, an intake buffer tank 18, an exhaust buffer tank 20, and a vacuum pump 8, and the high pressure resistant crystal petri dish 5 passes through the high pressure hose 9 respectively.
  • the intake buffer tank 18 is in communication with the exhaust buffer tank 20, and the high pressure hose 9 is respectively provided with an inlet needle valve 11 and an exhaust port needle valve 10, the intake buffer tank 18 and the A bypass needle valve 19 is disposed between the exhaust buffer tanks 20, and the vacuum pump 8 communicates with the exhaust port needle valve 10 through the vacuum pump needle valve 15, and the intake buffer tank 18 is provided with an intake buffer a tank pressure sensor 16 and an intake buffer tank thermocouple thermometer 17, the exhaust buffer tank 20 is provided with an exhaust buffer tank thermocouple thermometer 21 and an exhaust buffer tank pressure sensor 22;
  • the data acquisition system includes a thermocouple thermometer and a pressure sensor, and the mobile gantry 1 is provided with a paperless recorder 2, and the thermocouple thermometer and the pressure sensor transmit data to the paperless recorder 2
  • the precision positioning platform 14 is disposed in front of the high pressure resistant crystal culture dish 5, and the precision positioning platform 14 is provided with a camera 13.
  • the mobile gantry 1 adopts an aluminum alloy skeleton, and the rest are made of stainless steel plate materials.
  • the high pressure resistant crystal culture dish fixing bracket 5b is a hollow structure, and the low temperature thermostatic tank 3 passes through the cooling liquid hose 6 through the hollow structure of the high pressure resistant crystal culture dish fixing bracket 5b and the high pressure resistant crystal culture dish. 5 phases are connected.
  • the stage is a detachable component; the stage is made of brass and has a "work" shape structure; the upper end surface of the stage is covered with a layer of polytetrafluoroethylene material; the bottom of the stage The bottom wall of the high pressure resistant cavity is fitted and provided with a cylindrical positioning pin.
  • the elongated intake pipe is a detachable component; the extended intake pipe is made of stainless steel.
  • the two side glasses on the moving gantry 1 opposite to the high pressure resistant crystal petri dish 5 are electromagnetic liquid crystal dimming glasses.
  • the high-pressure resistant crystal petri dish 5 and the inner high-pressure resistant cavity 5x thereof have a flat cylindrical shape.
  • the gas hydrate crystal culture device is applied to the measurement experiment of crystal growth process of methane hydrate crystal at 2 ° C and 4 MPa, and its use method is described.
  • the methane gas used in the experiment came from Guangzhou Spectrum Source Gas Co., Ltd., and the purity was not less than 99.9%.
  • the water used to form the methane hydrate is distilled water and is prepared by a laboratory.
  • the general working process is divided into three parts: equipment assembly and injection, crystal growth observation and instrument finishing.
  • the high pressure hose 9 is first connected to the intake and exhaust ports of the high pressure resistant crystal petri dish 5 and the coolant hose 6 is connected.
  • the wiped clean high pressure resistant crystal petri dish window glass 5f was mounted on the high pressure resistant crystal petri dish body 5d and fixed and sealed with a high pressure resistant crystal petri dish window end cap 5e.
  • About 3 mL of pure water was injected into the high pressure resistant chamber through the incident laser window using a syringe, and then the wiped incident laser window glass 5c was attached and fixed and sealed with the incident laser window end cover 5a. Connect the power and check the imaging of the camera.
  • the observation chamber 4 is placed on the high pressure resistant crystal culture dish 5 and the incident angle of the laser light source is adjusted, so that the incident effect of the light source reaches an optimum level.
  • the paperless recorder 2 is first turned on, and it is checked whether the temperature and pressure values of the high pressure resistant crystal petri dish 5, the intake buffer tank 18, and the exhaust buffer tank 20 are significantly deviated from the normal temperature and normal pressure.
  • the temperature of the high pressure resistant crystal petri dish 5 is then controlled using a temperature control system. Turn on the circulation pump of the low temperature bath 3 and check the coolant circulation line for leaks.
  • the temperature of the cryostat 3 was set at 1 ° C and the refrigeration system was turned on. After the stabilization in the high pressure resistant crystal petri dish 5, the set temperature of the cryostat 3 was adjusted until the temperature was constant at 2 °C.
  • the pressure of the high pressure resistant crystal petri dish 5 is then adjusted using a pressure control system.
  • the high pressure gas source, the bypass needle valve 19, the vent needle valve 10 and the inlet needle valve 11 are opened, and the chambers in the intake buffer tank 18, the exhaust buffer tank 20, and the high pressure resistant crystal petri dish 5 are blown. sweep. Thereafter, the high pressure gas source is turned off and the vacuum pump needle valve 15 and the vacuum pump 8 are turned on to evacuate. After the temperature and pressure in the intake buffer tank 19, the exhaust buffer tank 20, and the high pressure resistant crystal petri dish 5 are stabilized, the vacuum pump needle valve 15 and the vacuum pump 8 are closed and slowly moved to the intake buffer tank 19 and the exhaust buffer tank 20 High pressure gas is injected into the high pressure crystal culture dish 5.
  • the gas hydrate crystal grows slowly in a static solution, so the crystal growth process needs to undergo a growth process of several hours or even several days.
  • the electromagnetic liquid crystal dimming glass is turned off to prevent The influence of external environmental radiation on the growth process of hydrate crystals.
  • the solution in the high pressure resistant chamber 5x is completely converted into a gas hydrate crystal
  • the gas hydrate crystal growth process is completed.
  • the temperature of the cryostat 3 was raised again to 8 ° C to completely decompose the gas hydrate in the high pressure resistant cavity 5x. Thereafter, the temperature in the high pressure resistant crystal petri dish 5 was again lowered to 2 ° C, and the gas hydrate formation process was observed again.
  • the growth process of the gas hydrates is substantially the same, the observation of the gas hydrate growth process is completed.
  • the temperature of the cryostat 3 is first raised to 8 ° C to completely decompose the gas hydrate therein. Then, the vent needle 10 and the bypass needle 19 on the vent buffer tank 20 are successively opened to slowly release the methane gas in the pressure vessel.
  • the cryostat 3 is adjusted to a temperature of 25 ° C and the cryostat 3 is turned off.
  • the electromagnetic liquid crystal dimming glass is opened and the observation bin 4 is opened, the incident laser window end cover 5a is unscrewed, the incident laser window glass 5c is taken out, and the solution in the high pressure resistant cavity is sucked out by a syringe.

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  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
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  • Metallurgy (AREA)
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  • Optics & Photonics (AREA)
  • Electromagnetism (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

一种气体水合物晶体培养装置，包括耐高压晶体培养皿（5）、温度控制系统、压力控制系统、数据采集系统和移动台架（1）。本装置通过改变耐高压晶体培养皿(5)中的实验配件即可完成鼓泡法、液滴法、溶液生长法等多种实验研究方法，提高了设备的通用性。其次，针对传统气体水合物晶体培养装置遇到的观测精度不高，装置耐压能力较低的情况，强化了水合物晶体培养皿围护结构对外界环境中热传导和热辐射的隔离效果，改良了水合物晶体培养皿内部背景光源的入射质量和入射方式，实现了摄像镜头的二维遥控移动，提高了水合物晶体培养皿的耐压和耐低温能力。这使得水合物晶体学测量更加精准，被用于水合物晶体测量的种类更加丰富。

Description

一种气体水合物晶体培养装置 技术领域
本发明涉及晶体培养设备技术领域，具体涉及一种气体水合物晶体培养装置。
背景技术
气体水合物是由气体分子和水分子组成的、形成于低温和高压条件下的具有笼状结构的似冰状结晶化合物。自然形成的气体水合物广泛分布于深海沉积物或者大陆永久冻土层中。近年来随着天然气水合物在全球范围内的大量发现，使其成为一种极具开发潜力的可替代能源而得到世界各国的重视。目前，在全球范围内已经探明的天然气水合物储量达到2.1×10 16m 3，是传统化石能源总量的两倍以上。与此同时，气体水合物的储气密度大。1标准体积的气体水合物可以存储高达160标准体积的气体。其存储所需的温度和压力条件又比液化气体温和，因此可以广泛应用于天然气储运和二氧化碳的固定与封存。因此，研究气体水合物的动力学特性和相关机理对于实现天然气水合物的开采、储运以及温室气体的捕集与封存具有十分重要的意义。
气体水合物在常温常压条件下处于不稳定状态，极易分解成气体和液态水。而维持水合物晶体结构稳定则需要较低的温度和较高的压力。例如在1℃下，保持甲烷气体水合物晶体稳定所需要的最低压力约为2.9MPa。因此，在室温和一个大气压的常规条件下难以完成水合物相关物性和晶体特性方面的测量。与此同时，气体水合物的多孔特性，非化学计量特性以及晶体结构对气体压力的敏感性导致单个气体水合物晶体难以生长成为肉眼可见的可测量的尺寸，使得对气体水合物进行的单晶测量更加困难，水合物晶体在溶液中的生长动力学特性的研究也无法开展。为了完成气体水合物在晶体学领域的研究与突破，必须对原有设备进行改进。
目前，国际上一些研究机构已经研发出相关的气体水合物晶体培养设备。这些设备可以完成4MPa和10℃以下的环境条件中，气体水合物晶体的生长动力学研究或者单晶制备。同时，由于晶体培养设备的容积较小，光源设置不合理等原因导致实验结果并不具有较好的说服力。因此，提高仪器的耐压能力，扩大仪 器在不同晶体学研究手段中的应用，改善气体水合物晶体培养设备中光源和拍摄设置，是实现气体水合物晶体结构的原位测量成为进一步展开气体水合物晶体学实验分析的重大难题。
发明内容
本发明提供一种气体水合物晶体培养装置，以期达到通用性的目地，使得测量更加精准的技术效果。
为实现上述目的，本发明的技术方案是：
一种气体水合物晶体培养装置，包括移动台架、温度控制系统、压力控制系统、数据采集系统和耐高压晶体培养皿，所述耐高压晶体培养皿、所述温度控制系统、所述压力控制系统和所述数据采集系统均安装于所述移动台架上；
所述耐高压晶体培养皿，包括耐高压晶体培养皿本体，所述耐高压晶体培养皿本体的上端设有入射激光窗口端盖，下端设有耐高压晶体培养皿固定支架，内部设有耐高压腔体，所述入射激光窗口端盖下方设有入射激光窗口玻璃，所述入射激光窗口玻璃两侧分别为所述耐高压腔体进气口和排气口，所述进气口连通加长进气管，所述耐高压腔体外侧设有冷却液夹套，冷却液的进口和出口位于冷却液夹套底部中央，所述耐高压腔体侧壁底部设有所述载物台，所述耐高压腔体两侧面对称分布耐高压腔体窗口玻璃，所述耐高压腔体窗口玻璃外设有耐高压腔体窗口端盖；
所述温度控制系统，包括低温恒温槽和冷却液软管，所述低温恒温槽通过所述冷却液软管与所述耐高压晶体培养皿相连通，所述耐高压晶体培养皿上端设有耐高压晶体培养皿热电偶温度计和耐高压晶体培养皿压力传感器；
所述压力控制系统，包括高压软管、真空泵针阀、进气缓冲罐、排气缓冲罐和真空泵，所述耐高压晶体培养皿通过所述高压软管分别与所述进气缓冲罐和所述排气缓冲罐相连通，所述高压软管上分别设有进气口针阀和排气口针阀，所述进气缓冲罐和所述排气缓冲罐之间设有旁通针阀，所述真空泵通过所述真空泵针阀与排气口针阀相连通，所述进气缓冲罐上设有进气缓冲罐压力传感器和进气缓冲罐热电偶温度计，所述排气缓冲罐上设有排气缓冲罐热电偶温度计和排气缓冲罐压力传感器；
所述数据采集系统，包括热电偶温度计和压力传感器，所述移动台架上设有无纸记录仪，所述热电偶温度计和所述压力传感器将数据传输到所述无纸记录仪上，所述耐高压晶体培养皿前方设有所述精密定位平台，所述精密定位平台上设有摄像头。
进一步地，所述移动台架采用铝合金骨架，其余均采用不锈钢板材料制成。
进一步地，所述耐高压晶体培养皿固定支架为中空结构，所述低温恒温槽通过所述冷却液软管经过所述耐高压晶体培养皿固定支架的中空结构与所述耐高压晶体培养皿相连通。
进一步地，所述载物台为可拆卸部件；所述载物台采用黄铜制作，呈“工”字形结构；所述载物台上端面包覆一层聚四氟乙烯材料；所述载物台底部贴合耐高压腔体的底部壁面并设有圆柱形定位销。
进一步地，所述加长进气管为可拆卸部件；所述加长进气管采用不锈钢材质制成。
进一步地，所述移动台架上与所述耐高压晶体培养皿相对的两个侧面玻璃采用电磁液晶调光玻璃。
进一步地，所述耐高压晶体培养皿及其内部的内部的耐高压腔体均呈扁圆柱形。
其有益效果在于：本发明结合当前水合物晶体学研究的实验手段，通过改变耐高压晶体培养皿中的实验配件即可完成鼓泡法、液滴法、溶液生长法等多种实验研究方法，提高了设备的通用性。其次，本发明针对传统气体水合物晶体培养装置遇到的观测精度不高，装置耐压能力较低的情况，强化了水合物晶体培养皿围护结构对外界环境中热传导和热辐射的隔离效果，改良了水合物晶体培养皿内部背景光源的入射质量和入射方式，实现了摄像镜头的二维遥控移动，提高了水合物晶体培养皿的耐压和耐低温能力。这使得水合物晶体学测量更加精准，被用于水合物晶体测量的种类更加丰富。
附图说明
图1是本发明的工作流程图；
图2是本发明的结构示意图；
图3是图2从A-A′的剖视图；
图4是耐高压晶体培养皿的外部结构示意图；
图5是耐高压晶体培养皿的内部结构示意图；
图6是耐高压腔体的结构示意图；
图中附图标记的含义：1、移动台架，2、无纸记录仪，3、低温恒温槽，4、观察仓，5、耐高压晶体培养皿，6、冷却液软管，7、耐高压晶体培养皿热电偶温度计，8、真空泵，9、高压软管，10、排气口针阀，11、进气口针阀，12、耐高压晶体培养皿压力传感器，13、摄像头，14、精密定位平台，15、真空泵针阀，16、进气缓冲罐压力传感器，17、进气缓冲罐热电偶温度计，18、进气缓冲罐，19、旁通针阀，20、排气缓冲罐，21、排气缓冲罐热电偶温度计，22、排气缓冲罐压力传感器，5a、入射激光窗口端盖，5b、耐高压晶体培养皿固定支架，5c、入射激光窗口玻璃，5d、耐高压晶体培养皿本体，5e、耐高压腔体窗口端盖，5f、耐高压腔体窗口玻璃，5x、耐高压腔体，5y、冷却液夹套。
具体实施方式
下面结合附图和具体实施方式对本发明的内容做进一步详细说明。
实施例1：
一种气体水合物晶体培养装置，包括移动台架1、温度控制系统、压力控制系统、数据采集系统和耐高压晶体培养皿5，所述耐高压晶体培养皿5、所述温度控制系统、所述压力控制系统和所述数据采集系统均安装于所述移动台架1上；
所述耐高压晶体培养皿5，包括耐高压晶体培养皿本体5d，所述耐高压晶体培养皿本体5d的上端设有入射激光窗口端盖5a，下端设有耐高压晶体培养皿固定支架5b，内部设有耐高压腔体5x，所述入射激光窗口端盖5a下方设有入射激光窗口玻璃5c，所述入射激光窗口玻璃5c两侧分别为所述耐高压腔体5x进气口和排气口，所述进气口连通加长进气管，所述耐高压腔体5x外侧设有冷却液夹套5y，冷却液的进口和出口位于冷却液夹套5y底部中央，所述耐高压腔体5x侧壁底部设有所述载物台，所述耐高压腔体5x两侧面对称分布耐高压腔体窗口玻璃5f，所述耐高压腔体窗口玻璃5f外设有耐高压腔体窗口端盖5e；
所述温度控制系统，包括低温恒温槽3和冷却液软管6，所述低温恒温槽3 通过所述冷却液软管6与所述耐高压晶体培养皿5相连通，所述耐高压晶体培养皿5上端设有耐高压晶体培养皿热电偶温度计7和耐高压晶体培养皿压力传感器12；
所述压力控制系统，包括高压软管9、真空泵针阀15、进气缓冲罐18、排气缓冲罐20和真空泵8，所述耐高压晶体培养皿5通过所述高压软管9分别与所述进气缓冲罐18和所述排气缓冲罐20相连通，所述高压软管9上分别设有进气口针阀11和排气口针阀10，所述进气缓冲罐18和所述排气缓冲罐20之间设有旁通针阀19，所述真空泵8通过所述真空泵针阀15与排气口针阀10相连通，所述进气缓冲罐18上设有进气缓冲罐压力传感器16和进气缓冲罐热电偶温度计17，所述排气缓冲罐20上设有排气缓冲罐热电偶温度计21和排气缓冲罐压力传感器22；
所述数据采集系统，包括热电偶温度计和压力传感器，所述移动台架1上设有无纸记录仪2，所述热电偶温度计和所述压力传感器将数据传输到所述无纸记录仪2上，所述耐高压晶体培养皿5前方设有所述精密定位平台14，所述精密定位平台14上设有摄像头13。
其中，所述移动台架1采用铝合金骨架，其余均采用不锈钢板材料制成。所述耐高压晶体培养皿固定支架5b为中空结构，所述低温恒温槽3通过所述冷却液软管6经过所述耐高压晶体培养皿固定支架5b的中空结构与所述耐高压晶体培养皿5相连通。所述载物台为可拆卸部件；所述载物台采用黄铜制作，呈“工”字形结构；所述载物台上端面包覆一层聚四氟乙烯材料；所述载物台底部贴合耐高压腔体的底部壁面并设有圆柱形定位销。所述加长进气管为可拆卸部件；所述加长进气管采用不锈钢材质制成。所述移动台架1上与所述耐高压晶体培养皿5相对的两个侧面玻璃采用电磁液晶调光玻璃。所述耐高压晶体培养皿5及其内部的内部的耐高压腔体5x均呈扁圆柱形。
以气体水合物晶体培养装置应用于甲烷水合物晶体在2℃，4MPa时晶体生长过程的测量实验为例，叙述其使用方法。实验用的甲烷气体来自广州谱源气体有限公司，纯度不低于99.9％。形成甲烷水合物所用的水为蒸馏水,由实验室制备。
其一般工作过程按时间先后顺序分为：设备组装与进样，晶体生长观测和仪器整理三个环节。
在设备组装与进样环节，首先将高压软管9与耐高压晶体培养皿5的进气和排气口相连接并连接冷却液软管6。将擦拭干净的耐高压晶体培养皿窗口玻璃5f安装在耐高压晶体培养皿本体5d上并用耐高压晶体培养皿窗口端盖5e固定和密封。利用注射器将约3mL的纯水通过入射激光窗口注入耐高压腔体中，然后安装擦拭干净的入射激光窗口玻璃5c并用入射激光窗口端盖5a固定和密封。连通电源并检查摄像头的成像效果。当对耐高压晶体培养皿5的安装与检查完毕后，将观察仓4盖在耐高压晶体培养皿5上并调节激光光源的入射角度，使光源入射效果达到最佳水平。
在晶体生长观测，首先开启无纸记录仪2，检查耐高压晶体培养皿5，进气缓冲罐18和排气缓冲罐20的温度和压力数值是否明显偏离常温常压。然后利用温度控制系统对耐高压晶体培养皿5的温度进行控制。开启低温恒温槽3的循环泵，检查冷却液循环管路是否存在漏液。将低温恒温槽3的温度设定在1℃并开启制冷系统。当耐高压晶体培养皿5中的稳定后，对低温恒温槽3的设定温度进行调节，直至温度恒定在2℃。随后利用压力控制系统对耐高压晶体培养皿5的压力进行调节。开启高压气源、旁通针阀19，排气口针阀10和进气口针阀11，对进气缓冲罐18、排气缓冲罐20和耐高压晶体培养皿5中的腔体进行吹扫。之后，关闭高压气源并开启真空泵针阀15和和真空泵8进行抽真空。当进气缓冲罐19、排气缓冲罐20和耐高压晶体培养皿5中的温度和压力稳定之后，关闭真空泵针阀15和和真空泵8并缓慢向进气缓冲罐19、排气缓冲罐20和耐高压晶体培养皿5中注入高压气体。当耐高压晶体培养皿5中压力达到3.8MPa时，关闭旁通针阀19和进气口针阀11并继续向进气缓冲罐19中进气使其压力达到6MPa。关闭高压气源并缓慢向开启进气口针阀11，继续向耐高压晶体培养皿5，使耐高压晶体培养皿5的压力达到设定值，最终关闭进气口针阀11。此时，耐高压晶体培养皿5中的溶液处于过饱和状态。此时，通过精密定位平台14调节摄像头的拍摄角度并开始录像。在通常情况下，气体水合物晶体在静止的溶液中生长过程较慢，因此晶体的生长过程需要经历几个小时甚至几天的生长过程，在晶体生长过程中，关闭电磁液晶调光玻璃，防止外界环境辐射对水合物晶体生长过程的影响。当耐高压腔体5x中的溶液完全转化成气体水合物晶体时，气体水合物晶体生长过程完成。将低温恒温槽3的温度再次上升至8℃，使耐高压腔体 5x中的气体水合物完全分解。之后再次将耐高压晶体培养皿5中的温度降至2℃，对气体水合物的生成过程进行再次观测。当两次气体水合物的生长过程基本一致后，完成对气体水合物生长过程的观测。
在仪器整理环节，首先将低温恒温槽3的温度上升至8℃，使其中的气体水合物完全分解。然后先后打开排气缓冲罐20上的排气口针阀10和旁通针阀19，使压力容器中的甲烷气体缓慢释放。当压力下降至大气压力时，调节低温恒温槽3设定温度至25℃并关闭低温恒温槽3。开启电磁液晶调光玻璃并打开观察仓4，旋开入射激光窗口端盖5a，取出入射激光窗口玻璃5c并用注射器吸出耐高压腔体中的溶液。最后，旋松耐高压晶体培养皿窗口端盖5e上的螺丝，依次取下耐高压晶体培养皿窗口端盖5e和耐高压晶体培养皿窗口玻璃5f并对耐高压晶体培养皿本体5d和耐高压晶体培养皿窗口玻璃5f进行清洁。最后，关闭无纸记录仪2，完成实验仪器的维护与整理。
上述实施例只是为了说明本发明的技术构思及特点，其目的是在于让本领域内的普通技术人员能够了解本发明的内容并据以实施，并不能以此限制本发明的保护范围。凡是根据本发明内容的实质所做出的等效的变化或修饰，都应涵盖在本发明的保护范围内。

Claims (7)

  1. 一种气体水合物晶体培养装置，其特征在于，包括移动台架(1)、温度控制系统、压力控制系统、数据采集系统和耐高压晶体培养皿(5)，所述耐高压晶体培养皿(5)、所述温度控制系统、所述压力控制系统和所述数据采集系统均安装于所述移动台架(1)上；
    所述耐高压晶体培养皿(5)，包括耐高压晶体培养皿本体(5d)，所述耐高压晶体培养皿本体(5d)的上端设有入射激光窗口端盖(5a)，下端设有耐高压晶体培养皿固定支架(5b)，内部设有耐高压腔体(5x)，所述入射激光窗口端盖(5a)下方设有入射激光窗口玻璃(5c)，所述入射激光窗口玻璃(5c)两侧分别为所述耐高压腔体(5x)进气口和排气口，所述进气口连通加长进气管，所述耐高压腔体(5x)外侧设有冷却液夹套(5y)，冷却液的进口和出口位于冷却液夹套(5y)底部中央，所述耐高压腔体(5x)侧壁底部设有所述载物台，所述耐高压腔体(5x)两侧面对称分布耐高压腔体窗口玻璃(5f)，所述耐高压腔体窗口玻璃(5f)外设有耐高压腔体窗口端盖(5e)；
    所述温度控制系统，包括低温恒温槽(3)和冷却液软管(6)，所述低温恒温槽(3)通过所述冷却液软管(6)与所述耐高压晶体培养皿(5)相连通，所述耐高压晶体培养皿(5)上端设有耐高压晶体培养皿热电偶温度计(7)和耐高压晶体培养皿压力传感器(12)；
    所述压力控制系统，包括高压软管(9)、真空泵针阀(15)、进气缓冲罐(18)、排气缓冲罐(20)和真空泵(8)，所述耐高压晶体培养皿(5)通过所述高压软管(9)分别与所述进气缓冲罐(18)和所述排气缓冲罐(20)相连通，所述高压软管(9)上分别设有进气口针阀(11)和排气口针阀(10)，所述进气缓冲罐(18)和所述排气缓冲罐(20)之间设有旁通针阀(19)，所述真空泵(8)通过所述真空泵针阀(15)与排气口针阀(10)相连通，所述进气缓冲罐(18)上设有进气缓冲罐压力传感器(16)和进气缓冲罐热电偶温度计(17)，所述排气缓冲罐(20)上设有排气缓冲罐热电偶温度计(21)和排气缓冲罐压力传感器(22)；
    所述数据采集系统，包括热电偶温度计和压力传感器，所述移动台架(1)上设有无纸记录仪(2)，所述热电偶温度计和所述压力传感器将数据传输到所述 无纸记录仪(2)上，所述耐高压晶体培养皿(5)前方设有所述精密定位平台(14)，所述精密定位平台(14)上设有摄像头(13)。
  2. 根据权利要求1所述气体水合物晶体培养装置，其特征在于，所述移动台架(1)采用铝合金骨架，其余均采用不锈钢板材料制成。
  3. 根据权利要求1所述气体水合物晶体培养装置，其特征在于，所述耐高压晶体培养皿固定支架(5b)为中空结构，所述低温恒温槽(3)通过所述冷却液软管(6)经过所述耐高压晶体培养皿固定支架(5b)的中空结构与所述耐高压晶体培养皿(5)相连通。
  4. 根据权利要求1所述气体水合物晶体培养装置，其特征在于，所述载物台为可拆卸部件；所述载物台采用黄铜制作，呈“工”字形结构；所述载物台上端面包覆一层聚四氟乙烯材料；所述载物台底部贴合耐高压腔体的底部壁面并设有圆柱形定位销。
  5. 根据权利要求1所述气体水合物晶体培养装置，其特征在于，所述加长进气管为可拆卸部件；所述加长进气管采用不锈钢材质制成。
  6. 根据权利要求1所述气体水合物晶体培养装置，其特征在于，所述移动台架(1)上与所述耐高压晶体培养皿(5)相对的两个侧面玻璃采用电磁液晶调光玻璃。
  7. 根据权利要求1所述气体水合物晶体培养装置，其特征在于，所述耐高压晶体培养皿(5)及其内部的内部的耐高压腔体(5x)均呈扁圆柱形。
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