CN108387704A - The decomposition of liquid nitrogen frozen gas hydrates sample and burner and its method - Google Patents

The decomposition of liquid nitrogen frozen gas hydrates sample and burner and its method Download PDF

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Publication number
CN108387704A
CN108387704A CN201810074858.0A CN201810074858A CN108387704A CN 108387704 A CN108387704 A CN 108387704A CN 201810074858 A CN201810074858 A CN 201810074858A CN 108387704 A CN108387704 A CN 108387704A
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sample chamber
sample
gas
liquid nitrogen
gas hydrates
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CN108387704B (en
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程思海
何赵
冯强强
邓剑锋
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Guangzhou Marine Geological Survey
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Guangzhou Marine Geological Survey
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/22Fuels; Explosives
    • G01N33/225Gaseous fuels, e.g. natural gas

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Abstract

The present invention provides decomposition and burner and its method of a kind of liquid nitrogen frozen gas hydrates sample, the decomposition and burner include sample chamber, balance cabin, air-out apparatus, regulating valve and methane detection instrument, the sample chamber is connected to the balance cabin, and the height in the balance cabin is more than the height of the sample chamber;Described air-out apparatus one end is connected to the sample chamber, and outlet nozzle is arranged in the other end of air-out apparatus;The regulating valve is arranged on the air-out apparatus, and below the outlet nozzle;Methane detection instrument one end is stretched into the sample chamber, and is connected to the sample chamber, and sealing device is provided between the methane detection instrument and the sample chamber.The present invention can by be stored in be mixed with liquid nitrogen freezing gas hydrates sample in nitrogen and gas hydrates sample detach, and simple in structure, easy to operate, dependable performance.

Description

The decomposition of liquid nitrogen frozen gas hydrates sample and burner and its method
Technical field
The present invention relates to the decomposition of liquid nitrogen frozen gas hydrates sample and field of combustion technology, specifically, being related to A kind of decomposition of liquid nitrogen frozen gas hydrates sample and burner and its method.
Background technology
Gas hydrates are also known as " combustible ice ", are distributed widely in the permafrost of halmeic deposit or land-based area, by day The crystalline material for the class ice-like that right gas is formed with water under the conditions of high pressure low temperature.Because of its appearance as ice and also meet fire it is i.e. flammable It burns, so also referred to as " combustible ice ".Its Resource Density is high, and distribution on global is extensive, has high resource value, thus becomes Oil and gas industry circle studies for a long period of time hot spot.Since gas hydrates are extremely easy in decomposition at normal temperatures and pressures, so laboratory preserves day Right gas hydrate sample needs to be put in freezen protective in liquid nitrogen (under normal pressure, liquid nitrogen temperature is -196 DEG C).
The purity of gas hydrates sample is an important indicator in research, and the survey of gas hydrates purity It is fixed, it needs to take out gas hydrates from liquid nitrogen, places to heat up in a container and decompose, heat up to it gas for decomposing and releasing Body ingredient is collected, for subsequent experimental determination;Or to the gas ignition that releases of decomposition, by burning severe degree Lai The preliminary purity for judging gas hydrates sample.
Therefore, when the gas hydrates of freezen protective take out in liquid nitrogen, a certain amount of liquid nitrogen can be carried, liquid nitrogen volatilization is released A large amount of nitrogen is released, these nitrogen can be mixed into the gas of gas hydrate dissociation release, to seriously affect subsequent grind Study carefully work.
Invention content
In order to overcome above-mentioned technical problem, the freezing gas water for being mixed with liquid nitrogen can will be stored in the present invention provides a kind of Close the decomposition of liquid nitrogen frozen gas hydrates sample that nitrogen and gas hydrates sample in object sample are detached and Burner and its method.
To achieve the goals above, the decomposition of liquid nitrogen frozen gas hydrates sample of the present invention and burning dress It sets, including sample chamber, balance cabin, air-out apparatus, regulating valve and methane detection instrument, the sample chamber connect with the balance cabin Logical, the height in the balance cabin is more than the height of the sample chamber;Described air-out apparatus one end is connected to the sample chamber, outlet Outlet nozzle is arranged in the other end of device;The regulating valve is arranged on the air-out apparatus, and below the outlet nozzle;Institute It states methane detection instrument one end to stretch into the sample chamber, and is connected to the sample chamber, the methane detection instrument and the sample Sealing device is provided between cabin.
Preferably, sealing cover is set between the methane detection instrument and the sample chamber, and the sealing cover is around the methane Described sample chamber one end of stretching into of survey meter is arranged for one week.
Preferably, the decomposition of the liquid nitrogen frozen gas hydrates sample and burner further include oxygen detection Instrument, oxygen detection instrument one end is stretched into the sample chamber, and is connected to the sample chamber, the oxygen detection instrument with it is described Sealing cover is set between sample chamber, and the sealing cover is arranged for one week around described sample chamber one end of stretching into of the oxygen detection instrument.
Preferably, the oxygen detection instrument and the methane detection instrument are located at the both sides of the air-out apparatus.
Preferably, the decomposition of the liquid nitrogen frozen gas hydrates sample and burner further include gas flow Meter, the gas flowmeter are arranged on the air-out apparatus, and below the regulating valve.
Preferably, the decomposition of the liquid nitrogen frozen gas hydrates sample and burner, further include communicating pipe, institute It states balance cabin to be connected to by communicating pipe with the sample chamber, the both ends of the communicating pipe are located at the balance cabin and the sample The lower end in product cabin.
Preferably, the balance cabin is arranged in parallel with the sample chamber, the balance bilge portion and the sample chamber bottom In same horizontal line.
Preferably, the decomposition of the liquid nitrogen frozen gas hydrates sample and burner further include pedestal, described Balance cabin bottom and the sample chamber bottom be fixedly installed respectively and the pedestal on.
The decomposition of liquid nitrogen frozen gas hydrates sample of the present invention and combustion method include the following steps:
Step 1: the gas hydrates sample for being mixed with liquid nitrogen is taken out in liquid nitrogen container, it is placed in sample chamber, and past sample Product fill water in cabin, at this point, the water surface in sample chamber and balance cabin is maintained at sustained height;
Step 2: covering the sealing cover on methane detection instrument, regulating valve is opened;Under same temperature and pressure, liquid nitrogen Boiling point is lower than the temperature of gas hydrate dissociation, is mixed with liquid nitrogen subsidiary in the gas hydrates sample of liquid nitrogen and volatilizees first At nitrogen, it is discharged from outlet nozzle after the water surface of emerging;
Step 3: with temperature rise, gas hydrates sample, which starts to decompose, releases methane gas, methane detector Detect methane concentration increase;At this point, closing regulating valve, gas hydrates sample is made to decompose the air accumulation of release in sample The top in cabin, with the increase of release gas, the pressure of sample chamber is consequently increased, and the water in sample chamber enters balance cabin, makes The water surface that must be balanced in cabin is higher than sample chamber, and pressure is provided for gas discharge;Wait for that gas hydrates sample does not have bubble generation When, gas hydrates sample decomposes completely;
Step 4: the atmospheric sampling bag vacuumized is connected with outlet nozzle, regulating valve is slowly opened, the gas at the top of sample chamber Body is collected by outlet nozzle in atmospheric sampling bag.
Preferably, the decomposition of the liquid nitrogen frozen gas hydrates sample and combustion method are further comprising the steps of:
Step 5: flow velocity when passing through outlet nozzle using gas flowmeter detection gas and total flow;
Step 6: having detected whether that oxygen is mixed into using oxygen detection instrument, it is then to be sealed operation;
It is no, then enter in next step;
Step 7: controlling the speed that gas flows out outlet nozzle by regulating valve, lighted, and makes the gas of collection can It burns under control state.
Technical solution provided by the present application can reach following advantageous effect:
For the present invention due under same temperature and pressure, the boiling point of liquid nitrogen is -196 DEG C, and gas hydrate dissociation Temperature is -45 DEG C, therefore is mixed with liquid nitrogen subsidiary in the gas hydrates sample of liquid nitrogen and is volatilized into nitrogen first, from outlet nozzle Discharge.In this way, the technical issues of just solving the gas that nitrogen can be mixed into gas hydrate dissociation release;Reach nitrogen With the technique effect of the gas phase separation of gas hydrate dissociation release;To ensure the gas hydrate dissociation being collected into The gas purity of release is higher, is conducive to subsequent research, and by controllable valve (i.e. regulating valve), and the gas of collection can be made can It burns under control state.
Description of the drawings
Fig. 1 is the structural representation of the decomposition and burner of liquid nitrogen frozen gas hydrates sample of the present invention Figure.
Specific implementation mode
Below with reference to the accompanying drawings illustrate the embodiment of the present invention.It is retouched in the attached drawing of the present invention or a kind of embodiment The elements and features stated can be combined with elements and features shown in one or more other drawings or embodiments.It answers When note that for purposes of clarity, being omitted known to unrelated to the invention, those of ordinary skill in the art in attached drawing and explanation Component or processing expression and description.
The present invention is described further below in conjunction with the accompanying drawings.
As shown in Figure 1, the decomposition of liquid nitrogen frozen gas hydrates sample of the present invention and burner include sample Product cabin 1, balance cabin 2, air-out apparatus 3, regulating valve 4 and methane detection instrument 5, the sample chamber is connected to the balance cabin, right When nitrogen after liquid nitrogen volatilization is detached with the gas that gas hydrate dissociation discharges, need to fill in sample chamber Water allows for sample chamber 1 and the water surface in balance cabin 2 relative to level in this way since sample chamber 1 is connected with balance cabin 2 The height in face is equal, and under same temperature and pressure, the boiling point of liquid nitrogen is -196 DEG C, and the temperature of gas hydrate dissociation It is -45 DEG C, so liquid nitrogen subsidiary in sample is volatilized into nitrogen first, the water surface of emerging.Since air-out apparatus 3 includes a rod-shaped knot Structure 31 and an outlet nozzle 32, wherein one end of rod-like structure 31 is connected to sample chamber 1, the other end and outlet of rod-like structure 31 Mouth 31 connects;Therefore, emerge the water surface nitrogen first from the outlet nozzle of air-out apparatus 31 be discharged.
Wherein, the height in the balance cabin 2 is more than the height of the sample chamber 1, due to being released in collection gas hydrates When releasing methane gas, a part of water in sample chamber can flow into balance cabin so that the water surface in balance cabin is higher than sample The water surface in product cabin, that is to say, that the pressure in sample chamber is more than the pressure in balance cabin, thus to subsequent collection natural gas Hydrate releases methane gas (main component of natural gas is methane) and provides pressure.
The regulating valve 4 is arranged on the air-out apparatus 3, and positioned at 32 lower section of the outlet nozzle;Regulating valve is for adjusting Save the flow that gas is discharged in decomposition or burning.Described 5 one end of methane detection instrument is stretched into the sample chamber 1, and with it is described Sample chamber 1 is connected to, and it is to manipulate regulating valve to detect methane for convenience of people that methane detection instrument is arranged herein.The first It is provided with sealing device between alkane survey meter 5 and the sample chamber 1.Sealing cover mentioned here can make sealing ring, gasket Or other similar devices that can play sealing function.In the present embodiment, sealing device is sealing cover 6.That is, the methane Sealing cover 6 is set between survey meter 5 and the sample chamber 1, and the sealing cover stretches into the sample around the methane detection instrument Cabin one end is arranged for one week.That is, when covering sealing cover 6, without the oxygen in air from methane detection instrument and sample Gap between product cabin enters in sample chamber.
In this way, with temperature rise, gas hydrates sample, which starts to decompose, releases methane gas, and methane detector can To be immediately detected methane concentration sharp increase.At this moment, regulating valve 4 is closed, keeps the gas that gas hydrates sample decomposes release poly- The top for combining in sample chamber 1, with the increase of release gas, the pressure of sample chamber 1 is consequently increased, and the water in sample chamber enters Balance cabin 2 so that the water surface in balance cabin is higher than sample chamber, and pressure is provided for gas discharge.
Wherein, the decomposition of the liquid nitrogen frozen gas hydrates sample and burner further include oxygen detection instrument 7, Oxygen detection instrument one end is stretched into the sample chamber, and is connected to the sample chamber 1, the oxygen detection instrument 7 with it is described Sealing cover 6 is set between sample chamber 1, and the sealing cover is set for one week around described sample chamber one end of stretching into of the oxygen detection instrument It sets.It is identical as the sealing cover on methane detection instrument, sealing cover herein be also prevent oxygen in air from oxygen detection instrument with Gap between sample chamber enters in sample chamber.
It should be noted that:Herein setting oxygen detection instrument be in order to gas hydrates discharge methane when, It has detected whether that oxygen is mixed into, if there is oxygen is mixed into, then has just needed to detect whether sealing cover covers tightly, if mixed without oxygen Enter, then can carry out it is subsequent light, when also avoiding to be mixed into oxygen in methane, lighting can there is a situation where explode to occur.
Wherein, in the present embodiment, the oxygen detection instrument 7 and the methane detection instrument 5 are located at the outlet dress The both sides set.In this way, people is facilitated especially to exist the operation of oxygen detection instrument and methane detection instrument to a certain extent When oxygen detection instrument and methane detection instrument work at the same time.
Wherein, the decomposition of liquid nitrogen frozen gas hydrates sample and burner further include gas flowmeter 8, the gas Flowmeter body 8 is arranged on the air-out apparatus 3, and positioned at 4 lower section of the regulating valve.Setting gas flowmeter 8 can herein Flow velocity to be measured to the gas volume that gas hydrate dissociation discharges, and when showing gas by outlet nozzle 32 and total Flow.In this way, also people is facilitated to the operation of regulating valve, that is, to be beaten on the basis of flow velocity and flow number to a certain extent Open and close are closed or are tuned up, turn down.
Wherein, in the present embodiment, the balance cabin is connected to the sample chamber by a connecting pipe 9, by It is a simple communication apparatus in communicating pipe, therefore, it is more simple to allow for apparatus structure in this way, facilitates people to device Operation.The both ends of communicating pipe 9 described herein are located at the lower end in the balance cabin and the sample chamber, so that balance Cabin is connected to sample chamber in bottom, ensures that the gas of gas hydrate dissociation release is all collected in sample chamber in this way It is interior, without being diffused into balance cabin.
Certainly, in the embodiment other than the present invention, balance cabin can also be made directly to be connected to sample chamber, or will be even The both ends of siphunculus are integrated with sample chamber and the setting of balance cabin respectively.
Wherein, in the present embodiment, the balance cabin is arranged in parallel with the sample chamber, the balance bilge portion with it is described Sample chamber bottom is located in same horizontal line, in this way, when gas hydrates discharge methane, it is more convenient to make to put down Weigh cabin and sample chamber formation pressure difference, to which methane gas is pressed into air-out apparatus, and is discharged from outlet nozzle.
In the present embodiment, the decomposition of liquid nitrogen frozen gas hydrates sample and burner further include pedestal 10, institute State balance cabin bottom and the sample chamber bottom be fixedly installed respectively and the pedestal on.In this way, being in order to sample Product cabin and balance cabin are fixed.
The decomposition of liquid nitrogen frozen gas hydrates sample of the present invention and combustion method include the following steps:
Step 1: the gas hydrates sample for being mixed with liquid nitrogen is taken out in liquid nitrogen container, it is placed in sample chamber, and past sample Product fill water in cabin, at this point, the water surface in sample chamber and balance cabin is maintained at sustained height;
Step 2: covering the sealing cover on methane detection instrument, regulating valve is opened;Under same temperature and pressure, liquid nitrogen Boiling point is -196 DEG C, and the temperature of gas hydrate dissociation is -45 DEG C, i.e., the boiling point of liquid nitrogen is than gas hydrate dissociation Temperature is low, is mixed with liquid nitrogen subsidiary in the gas hydrates sample of liquid nitrogen and is volatilized into nitrogen first, from outlet after the water surface of emerging Mouth is discharged;
Step 3: with temperature rise, gas hydrates sample, which starts to decompose, releases methane gas, methane detector Methane concentration sharp increase can be immediately detected;At this point, closing regulating valve, keep the gas that gas hydrates sample decomposes release poly- The top for combining in sample chamber, with the increase of release gas, the pressure of sample chamber is consequently increased, and the water in sample chamber enters flat Weighing apparatus cabin so that the water surface in balance cabin is higher than sample chamber, and pressure is provided for gas discharge;Wait for that gas hydrates sample does not have gas When bubble generates, gas hydrates sample decomposes completely;
Step 4: the atmospheric sampling bag vacuumized is connected with outlet nozzle, regulating valve is slowly opened, the gas at the top of sample chamber Body is collected by outlet nozzle in atmospheric sampling bag.
Preferably, the decomposition of the liquid nitrogen frozen gas hydrates sample and combustion method are further comprising the steps of:
Step 5: flow velocity when passing through outlet nozzle using gas flowmeter detection gas and total flow;
Step 6: having detected whether that oxygen is mixed into using oxygen detection instrument, it is then to be sealed operation;
It is no, then enter in next step;
Step 7: controlling the speed that gas flows out outlet nozzle by regulating valve, lighted, and makes the gas of collection can It burns under control state.
The present invention the decomposition of liquid nitrogen frozen gas hydrates sample and the operation principle of burner be:
Gas hydrates sample is taken out in liquid nitrogen container, is placed in sample chamber, water is filled, at this moment sample chamber and balance The water surface in cabin is contour.Sealing cover is covered, regulating valve is opened.Under same temperature and pressure, the boiling point of liquid nitrogen is -196 DEG C, and The temperature of gas hydrate dissociation is -45 DEG C, so liquid nitrogen subsidiary in sample is volatilized into nitrogen first, after the water surface of emerging from Outlet nozzle is discharged.Then as temperature rise, gas hydrates sample, which starts to decompose, releases methane gas, methane detector Methane concentration sharp increase can be immediately detected.At this moment, regulating valve is closed, keeps the gas that gas hydrates sample decomposes release poly- The top for combining in sample chamber, with the increase of release gas, the pressure of sample chamber is consequently increased, and the water in sample chamber passes through company Siphunculus enters balance cabin so that the water surface in balance cabin is higher than sample chamber, and pressure is provided for gas discharge.Wait for gas hydrates When sample does not have bubble generation, you can think that it is decomposed completely.At this moment the atmospheric sampling bag and outlet that can will be vacuumized Mouth connects, and slowly opens regulating valve, and the gas at the top of sample chamber is collected into atmospheric sampling bag by outlet nozzle and is ground for subsequent Study carefully use, gas flowmeter can show flow velocity and total flow when gas passes through outlet nozzle.Gas is lighted if necessary, can be led to The speed for overregulating valve control gas outflow outlet nozzle, can burn in air.Gone out due to gas hydrate dissociation Gas componant is mainly methane, there is the possibility of explosion if when being mixed into oxygen and lighting.For this purpose, being visited equipped with oxygen on sealing cover Instrument is surveyed, can detect whether that oxygen is mixed into, to ensure the safety of operation.
Although the present invention and its advantage has been described in detail it should be appreciated that without departing from by the attached claims Defined by can carry out various changes, replacement and transformation in the case of the spirit and scope of the present invention.Moreover, the model of the application Enclose the specific embodiment for being not limited only to process, equipment, means, method and steps described in specification.In the art is common Technical staff executes and corresponding reality described herein from the disclosure it will be readily understood that can be used according to the present invention Apply the essentially identical function of example or obtain the result essentially identical with it, existing and process to be developed in future, equipment, Means, method or step.Therefore, the attached claims are intended to include such process, equipment, hand in the range of them Section, method or step.

Claims (10)

1. decomposition and the burner of a kind of liquid nitrogen frozen gas hydrates sample, which is characterized in that including sample chamber, balance Cabin, air-out apparatus, regulating valve and methane detection instrument, the sample chamber are connected to the balance cabin, the height in the balance cabin More than the height of the sample chamber;Described air-out apparatus one end is connected to the sample chamber, and the other end of air-out apparatus is provided Gas nozzle;The regulating valve is arranged on the air-out apparatus, and below the outlet nozzle;It stretches methane detection instrument one end Enter in the sample chamber, and be connected to the sample chamber, sealing dress is provided between the methane detection instrument and the sample chamber It sets.
2. decomposition and the burner of liquid nitrogen frozen gas hydrates sample according to claim 1, which is characterized in that Sealing cover is set between the methane detection instrument and the sample chamber, and the sealing cover is described around stretching into for the methane detection instrument Sample chamber one end is arranged for one week.
3. decomposition and the burner of liquid nitrogen frozen gas hydrates sample according to claim 1, which is characterized in that Further include oxygen detection instrument, oxygen detection instrument one end is stretched into the sample chamber, and is connected to the sample chamber, the oxygen Sealing cover is set between gas survey meter and the sample chamber, and the sealing cover stretches into the sample chamber around the oxygen detection instrument One end is arranged for one week.
4. decomposition and the burner of liquid nitrogen frozen gas hydrates sample according to claim 3, which is characterized in that The oxygen detection instrument and the methane detection instrument are located at the both sides of the air-out apparatus.
5. decomposition and the burner of liquid nitrogen frozen gas hydrates sample according to claim 1, which is characterized in that Further include gas flowmeter, the gas flowmeter is arranged on the air-out apparatus, and below the regulating valve.
6. decomposition and the burner of liquid nitrogen frozen gas hydrates sample according to claim 1, which is characterized in that It further include communicating pipe, the balance cabin is connected to the sample chamber by communicating pipe, and the both ends of the communicating pipe are located at institute State the lower end in balance cabin and the sample chamber.
7. the decomposition of the liquid nitrogen frozen gas hydrates sample and burning dress according to any one of claims 1 to 6 It sets, which is characterized in that the balance cabin is arranged in parallel with the sample chamber, the balance bilge portion and sample chamber bottom position In in same horizontal line.
8. decomposition and the burner of liquid nitrogen frozen gas hydrates sample according to claim 7, which is characterized in that Further include pedestal, it is described balance cabin bottom and the sample chamber bottom be fixedly installed respectively and the pedestal on.
9. decomposition and the combustion method of a kind of liquid nitrogen frozen gas hydrates sample, which is characterized in that include the following steps:
1) the gas hydrates sample for being mixed with liquid nitrogen is taken out in liquid nitrogen container, is placed in sample chamber, and noted into sample chamber Full water, at this point, the water surface in sample chamber and balance cabin is maintained at sustained height;
2) sealing cover on methane detection instrument is covered, regulating valve is opened;Under same temperature and pressure, the boiling point of liquid nitrogen is than natural The temperature that gas hydrate decomposes is low, is mixed with liquid nitrogen subsidiary in the gas hydrates sample of liquid nitrogen and is volatilized into nitrogen first, emits It is discharged from outlet nozzle after going out the water surface;
3) with temperature rise, gas hydrates sample, which starts to decompose, releases methane gas, and methane detector detects first Alkane concentration increases;At this point, closing regulating valve, gas hydrates sample is made to decompose the air accumulation of release in the top of sample chamber End, with the increase of release gas, the pressure of sample chamber is consequently increased, and the water in sample chamber enters balance cabin so that balance The water surface in cabin is higher than sample chamber, and pressure is provided for gas discharge;When gas hydrates sample does not have bubble generation, naturally Gas hydrate sample decomposes completely;
4) the atmospheric sampling bag vacuumized is connected with outlet nozzle, slowly opens regulating valve, the gas at the top of sample chamber is by going out Gas nozzle is collected into atmospheric sampling bag.
10. the decomposition of liquid nitrogen frozen gas hydrates sample according to claim 9 and combustion method, feature exist In further comprising the steps of after step 4):
5) flow velocity when passing through outlet nozzle using gas flowmeter detection gas and total flow;
6) it has detected whether that oxygen is mixed into using oxygen detection instrument, has been, be then sealed operation;
It is no, then enter in next step;
7) speed that gas flows out outlet nozzle is controlled by regulating valve, is lighted, and make the gas of collection under controllable state Burning.
CN201810074858.0A 2018-01-25 2018-01-25 Decomposing and burning device and method for liquid nitrogen frozen natural gas hydrate sample Active CN108387704B (en)

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