CN108587712A - A kind of synthetic method of high saturation hydrate - Google Patents
A kind of synthetic method of high saturation hydrate Download PDFInfo
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- CN108587712A CN108587712A CN201810391675.1A CN201810391675A CN108587712A CN 108587712 A CN108587712 A CN 108587712A CN 201810391675 A CN201810391675 A CN 201810391675A CN 108587712 A CN108587712 A CN 108587712A
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- hydrate
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- brine
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- 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
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- 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
- B01J10/00—Chemical processes in general for reacting liquid with gaseous media other than in the presence of solid particles, or apparatus specially adapted therefor
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- 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
- B01J19/002—Avoiding undesirable reactions or side-effects, e.g. avoiding explosions, or improving the yield by suppressing side-reactions
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- 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
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/02—Feed or outlet devices; Feed or outlet control devices for feeding measured, i.e. prescribed quantities of reagents
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of synthetic methods of high saturation hydrate, include the following steps：Prepare porous media model；Reaction kettle is vacuumized, brine is then injected into porous media model, until the brine in porous media model reaches saturation；Go out certain brine to reaction kettle note portion of methane gas drive, replaces part brine with methane gas, close outlet valve；Continue to note methane gas to reaction kettle, until reaching predetermined volume；Reaction kettle cooling synthesized hydrate；Repeat multiple injection gas, hydrate multi-stage synthesis to generate high saturation hydrate Tibetan.Accurate measurement is carried out to water filling volume by constant-flux pump, passes through the gas volume of flow controller metering injection；The volume of water filling gas injection can accurate measurement and monitoring in real time, the hydrate concentration being calculated is accurate.
Description
Technical field
The present invention relates to the synthesis technical fields of gas hydrates, and in particular to a kind of synthesis of high saturation hydrate
Method.
Background technology
Human society is faced with the resource exhaustion to become increasingly conspicuous and environmental disruption problem at present, and countries in the world all have adjusted energy
Source strategy arrangement, it may be found that with exploitation using the new energy of clean and effective as the top priority for solving the problems, such as future source of energy.It
Right gas hydrate is the class ice solid chemical compound formed under the conditions of cryogenic high pressure by natural gas and water.Global gas hydrates
Potential reserve be about 1.5 × 1016m3, it is widely distributed in land and ocean, stock number is abundant, and phosphorus content is high.It is estimated that from
The phosphorus content of hydrate is the 2 times or more of fossil fuel phosphorus content known to the whole world in right boundary.Divide since gas hydrates have
The characteristics of cloth is in extensive range, fuel value is high and cleanliness without any pollution, being considered 21 century most has the new energy of development prospect.
In general, the gas hydrates of nature are primarily present in the geological conditions such as permafrost area and deep seafloor
Extremely complex region it is big and of high cost to be sampled research difficulty, so indoor physics mould to hydrates Tibetan in these areas
Draft experiment is still one of the important means of research hydrate.And when studying hydrate basic characteristic, development scheme, it needs first
To do is to synthesize the hydrate similar with occurrence status under natural conditions.It is poor that presently found hydrate hides hydrate concentration
It is different larger, if the saturation degree of wheat rope Ahab hydrate concentration about 40%, and Alaska north slope hydrate Tibetan is up to 85%, I
The hydrate of state's Shenhu sea area hides saturation degree in 26%-48%.Therefore, synthesis high saturation hydrate is for studying hydrate phase
It is necessary to close property, development scheme etc..
Currently, the synthesis mode that the porous media model containing hydrate mostly uses disposable gas injection water filling is made, this conjunction
Generally be difficult to synthesize the hydrate of high saturation at mode, and hydrate generate after in reaction kettle can remaining many Free waters and from
By gas.If in addition, thinking to synthesize the hydrate of high saturation in this way, bulk gas, reaction kettle must be disposably injected
Pressure can be very big, and danger coefficient is higher.
Invention content
The present invention provides a kind of synthetic method of high saturation hydrate, this method cools down in general water filling gas injection to be synthesized
On the basis of hydrate, using multiple injection gas, gradually synthetic method, the gas hydrates for generating high saturation are realized.This
Invent it is highly practical, operation it is feasible, for physical simulation experiment research high saturation hydrate hide development approach and production
Dynamic is of great significance.
The technical solution of the use of the present invention is as follows：
Step 1 prepares porous media model in a kettle；
Specifically, quartz sand is cleaned repeatedly, waits for inserting reaction kettle after quartz sand drying, successively tamp, form densification
Uniform porous media model；
Resistivity test point, pressure-measuring-point, temperature point are equipped on two-dimensional flat plate porous media model, for measuring hydration
Object generates the dynamic changing process with resistivity, pressure, temperature in decomposable process, to analyze the generation of hydrate and decompose feelings
Condition；
Step 2 vacuumizes reaction kettle, and brine is then injected into porous media model, until in porous media model
Brine reaches saturation；
Specifically, being vacuumized first to reaction kettle, the gas in reaction kettle is discharged；Then open reaction kettle outlet valve and
Inlet valve injects certain density brine, when arrival end is noted with certain flow rate from inlet valve by constant-flux pump to reaction kettle
Water speed and outlet end production water speed are equal and after reaching and stablizing, it is believed that porous media model saturated brine.Close inlet valve
Door stops injection brine；
Step 3 goes out certain brine to reaction kettle note portion of methane gas drive, replaces part brine with methane gas, closes outlet
Valve；
Specifically, by reaction kettle entrance by water filling port changing-over to gas injection port, by gas cylinder into porous media model
High-purity methane gas is injected, after displacing the brine of certain volume, stops gas injection and closes outlet valve；
Step 4 continues to note methane gas to reaction kettle, until reaching predetermined volume；
Specifically, opening inlet valve, high-purity methane gas is injected into porous media model with constant gas injection speed,
By the methane gas volume of gas flow controller metering injection, predetermined volume to be achieved stops gas injection, closes inlet valve
And gas cylinder valve；At this time because injecting a large amount of methane gas, reacting kettle inner pressure increases.
Step 5 reaction kettle cooling synthesized hydrate；
Specifically, opening the thermostatic power and refrigeration power supply of reaction kettle, thermostat temperature is set, the appearances cooling synthesis such as carries out,
And record temperature, pressure, change in resistance in cooling building-up process；With the generation of hydrate, reacting kettle inner pressure gradually drops
Low, temperature is reduced to basicly stable after incubator set point temperature, and resistivity increases with increasing for hydrate quantity is generated.When more
When pressure, temperature, resistivity are stabilized to some value and no longer change substantially in the dielectric model of hole, illustrate that the stage hydrate closes
At completion.
(6) it repeats step (4-5) and carries out multiple injection gas, hydrate multi-stage synthesis to generate high saturation hydrate Tibetan.
Further, the computational methods for the hydrate concentration that the present invention obtains are as follows：
Saturation computation uses volume conservation method.Assuming that porous media model initial temperature and pressure are T1、P1, after synthesis
Porous media model temperature and pressure becomes T2、P2.Because NGH be etc. appearances synthesis, synthesize before water, gas volume should be equal to close
The volume of Cheng Houshui, gas, NGH, i.e.,：
V=Vw1+Vg1=Vw2+Vg2+Vh2 (1)
In formula, V is total pore volume, ml；Vw1、Vg1For initial temperature T1, pressure P1The volume of lower water, gas, ml；Vw2、
Vg2、Vh2For temperature T after synthesis2, pressure P2Lower water, gas and water close the volume of object, ml.
Assuming that the water and NGH of generation is incompressible and the NGH of unit volume decomposes the CH that can generate 164 unit volumes4Gas
Body.If shared Vgs cm3(under mark condition) CH4Reaction is converted into NGH, then above formula is represented by：
Abbreviation can obtain：
In formula, Z1、Z2Forward and backward compressibility factor is generated for hydrate；ρgFor methane air tightness under the status of criterion,
0.000715g/cm3；ρhFor methane hydrate density, 0.875g/cm3。ρwFor the density of water, 1.0g/cm3。
Then NGH saturation degrees ShFor：
Beneficial effects of the present invention are：
(1) method generated by multiple injection gas provides a kind of synthesis side of new feasible high saturation hydrate
Method；
(2) accurate measurement is carried out to water filling volume by constant-flux pump, passes through the gas volume of flow controller metering injection；
The hydrate concentration that can be calculated by above-mentioned formula (4)；
(3) since the method using multiple injection gas, stage generate hydrate, reactor pressure rises after each gas injection,
Reacting kettle inner pressure reduces after hydrate generates, therefore the pressure of reaction kettle is far below during this experimental method generation hydrate
The pressure-resistant limit, safety coefficient are high.
Description of the drawings
The accompanying drawings which form a part of this application are used for providing further understanding of the present application, and the application's shows
Meaning property embodiment and its explanation do not constitute the improper restriction to the application for explaining the application.
Fig. 1 is two-dimensional flat plate porous media model of the present invention, i.e. reaction kettle；
Fig. 2 is the structural schematic diagram of high saturation lanthanum chloride hydrate experimental provision of the present invention.
Wherein：1-fluid inlet, 2-resistivity test points, 3-pressure-measuring-points, 4-fluid outlets, 5 temperature points, 6-
Methane gas cylinder, 7-input end electronic balances and container, 8-constant-flux pumps, 9-intermediate receptacles, 10-insulating boxs, 11-back-pressure valves,
12-nitrogen cylinders, 13-output gases, 14-outlet end gas flowmeters, 15-outlet end electronic balances and container, 16-gas
Liquid/gas separator, 17-two-dimensional flat plate porous media models, 18-input end gas flowmeters, 19-valves.
Specific implementation mode
It is noted that following detailed description is all illustrative, it is intended to provide further instruction to the application.Unless another
It indicates, all technical and scientific terms used herein has usual with the application person of an ordinary skill in the technical field
The identical meanings of understanding.
It should be noted that term used herein above is merely to describe specific implementation mode, and be not intended to restricted root
According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singulative
It is also intended to include plural form, additionally, it should be understood that, when in the present specification using term "comprising" and/or " packet
Include " when, indicate existing characteristics, step, operation, device, component and/or combination thereof；
As background technology is introduced, the porous media model containing hydrate is made in the prior art and is mostly used disposably
The synthesis mode of gas injection water filling, this synthesis mode are generally difficult to synthesize the hydrate of high saturation, and anti-after hydrate generation
Answer in kettle that there are still more Free water and free gas.If, must in addition, think to synthesize the hydrate of high saturation in this way
Bulk gas must be disposably injected, pressure can be very big in model, and danger coefficient is higher.In order to solve technical problem as above,
Present applicant proposes a kind of synthetic methods of high saturation hydrate.
In a kind of typical embodiment of the application, as shown in Figure 1, being two-dimensional flat plate porous media model 17 of the present invention
Schematic diagram；One side is fluid inlet 1, and the other side is fluid outlet 4, and electricity is equipped on two-dimensional flat plate porous media model
Resistance rate measuring point 2, pressure-measuring-point 3, temperature point 5；It is generated and resistivity, pressure, temperature in decomposable process for measuring hydrate
Dynamic changing process, to analyze hydrate generation and decompose situation；Resistivity test point 2, pressure-measuring-point 3, temperature point 5
It is connected with presentation of information and processing equipment.
As shown in Fig. 2, whole synthesis system, including an insulating box 10, place two-dimensional flat plate in the inside of insulating box
The fluid inlet side of porous media model 17 (i.e. reaction kettle), two-dimensional flat plate porous media model 17 is filled by piping connection water source
It sets and compressed air source unit；The fluid outlet side of two-dimensional flat plate porous media model 17 passes through piping connection gas-liquid separator 16, gas-liquid
Separator 16 connects gas collector 13 and fluid collection device 15, and fluid collection device 15 is mounted on a weighing balance
On.
The water source device includes electronic balance and container 7, and the brine in container is pumped into two-dimensional flat plate by constant-flux pump
In porous media model 17, can also connect intermediate receptacle 9 and inlet valve on the pipeline；
The compressed air source unit includes methane gas cylinder 6, and methane gas cylinder 6 passes through piping connection two-dimensional flat plate porous media model
17,19 and gas flow meter 18 of inlet valve also is provided on the pipeline；
Gas-liquid separator 16 connects gas collector 13, and gas flowmeter 14 is additionally provided on connecting line；
The outlet of two-dimensional flat plate porous media model 17 is also connected with back-pressure valve 11 and outlet valve, and back-pressure valve 11 connects nitrogen
Bottle 12.
Specifically, the synthetic method of hydrate is described in detail with reference to specific numerical value：
(1) porous media model is prepared：By the quartz sand of 30-80 mesh 3-5 times wash with distilled water, inserted after drying flat
Slab is successively tamped, and the porous media model 17 of dense uniform is formed；17 size of flat plate model is 350 × 350 × 60mm,
Porosity is 0.35 after back-up sand.
Resistivity test point, pressure-measuring-point, temperature point are equipped on two-dimensional flat plate porous media model；For measuring hydration
Object generates the dynamic changing process with resistivity, pressure, temperature in decomposable process, to analyze the generation of hydrate and decompose feelings
Condition；
(2) reaction kettle is vacuumized, saturated water.It vacuumizes first, then opens two-dimensional flat plate porous media model 17
Outlet valve, from inlet valve by constant-flux pump 8 with 15ml/min to the brine of reaction kettle implantation quality a concentration of 3.5%, when
When outlet production water speed is equal with waterflood injection rate, it is believed that fully saturated brine, closing inlet valve amount to injection in model
1592ml brine.
(3) gas drive water.By model entrance by water filling port changing-over to gas injection port, height is injected into model by gas cylinder 6
Purity methane gas after displacing the brine of certain volume, stops gas injection and closes outlet side valve；
Herein, the concentration requirement of the high concentration methane gas is 99.9%.
(4) gas injection.CH is injected into model by gas injection port with the gas injection speed of 1SL/min4, use gas flow controller
The gas volume of 18 metering injections, stops gas injection when gas injection reaches 90000ml, closes gas injection port valve and gas cylinder, record this
When pressure p0=9.05Mpa, temperature T1=27.4 DEG C.
(5) cooling synthesis.Insulating box power supply and refrigeration power supply are opened, set 10 temperature of insulating box as 1 DEG C, the appearances such as carries out and drops
Temperature synthesis, and observe temperature, pressure, change in resistance in cooling building-up process；When pressure, temperature, resistivity are steady in model
When arriving some value surely and no longer changing substantially, illustrate that the stage lanthanum chloride hydrate is completed.Record pressure p at this time2=3.05Mpa,
Temperature T2=1.01 DEG C.The hydrate concentration S of stage synthesis can be calculated by equi-volume processH=16.1%
(6) the 2nd gas injections, the same step of method (4).Stage gas injection 53450ml, pressure p after gas injection3=
5.90Mpa, temperature T3=1.1 DEG C.
(7) synthesized hydrate, insulating box 10 maintain always 1 DEG C, remaining same step (5).Pressure at the end of lanthanum chloride hydrate
p4=2.98Mpa, temperature T4=0.95 DEG C, the hydrate concentration S of stage synthesis is calculatedH=11.5%
(8) step (6) and (7) is repeated several times, carries out gas injection altogether and synthesizes 5 times, finally obtained hydrate concentration is
64%.The hydrate concentration that temperature, pressure and each stage calculate before and after specific gas injection rate, gas injection is as shown in the table.
1 high saturation lanthanum chloride hydrate experimental data table of table
The foregoing is merely the preferred embodiments of the application, are not intended to limit this application, for the skill of this field
For art personnel, the application can have various modifications and variations.Within the spirit and principles of this application, any made by repair
Change, equivalent replacement, improvement etc., should be included within the protection domain of the application.
Claims (7)
1. a kind of synthetic method of high saturation hydrate, which is characterized in that include the following steps：
Step 1 prepares porous media model in a kettle；
Step 2 vacuumizes reaction kettle, and brine is then injected into porous media model, until the brine in porous media model
Reach saturation；
Step 3 goes out certain brine to reaction kettle note portion of methane gas drive, replaces part brine with methane gas, closes outlet valve
Door；
Step 4 continues to note methane gas to reaction kettle, until reaching predetermined volume；
Step 5 reaction kettle cooling synthesized hydrate；
Step 6 repeats step (4) to step (5) and carries out multiple injection gas, hydrate multi-stage synthesis to generate high saturation hydrate
It hides.
2. a kind of synthetic method of high saturation hydrate as described in claim 1, which is characterized in that the specific mistake of step 1
Cheng Shi：Quartz sand cleaning is multiple, it waits for inserting reaction kettle after quartz sand drying, successively tamps, form the porous of dense uniform
Dielectric model.
3. a kind of synthetic method of high saturation hydrate as described in claim 1, which is characterized in that the specific mistake of step 2
Cheng Shi：Reaction kettle is vacuumized first, the gas in reaction kettle is discharged；Then reaction kettle outlet valve and inlet valve are opened,
Certain density brine is injected to reaction kettle with certain flow rate from inlet valve by constant-flux pump, when the salt in porous media model
After water saturation, stops injection brine, close inlet valve.
4. a kind of synthetic method of high saturation hydrate as described in claim 1, which is characterized in that the specific mistake of step 3
Cheng Shi：By reaction kettle entrance by water filling port changing-over to gas injection port, high-purity is injected into porous media model by gas cylinder
Methane gas after displacing the brine of certain volume, stops gas injection and closes outlet valve.
5. a kind of synthetic method of high saturation hydrate as described in claim 1, which is characterized in that the specific mistake of step 4
Cheng Shi：Inlet valve is opened, high-purity methane gas is injected into porous media model with constant gas injection speed, passes through gas stream
The methane gas volume of amount controller metering injection, predetermined volume to be achieved stop gas injection, close inlet valve and bottle valve
Door.
6. a kind of synthetic method of high saturation hydrate as described in claim 1, which is characterized in that the specific mistake of step 5
Cheng Shi：The thermostatic power and refrigeration power supply for opening reaction kettle, set thermostat temperature, the appearances cooling synthesis such as carry out, and record cooling
Temperature, pressure, change in resistance in building-up process；When pressure, temperature, resistivity are stabilized to some in porous media model
When value no longer changes substantially, illustrate that the stage lanthanum chloride hydrate is completed.
7. a kind of synthetic method of high saturation hydrate as described in claim 1, which is characterized in that the specific mistake of step 6
Cheng Shi：As needed, step 4 and step 5 is repeated several times, to reach required hydrate concentration.
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| CN109628183A (en) * | 2018-12-18 | 2019-04-16 | 中国科学院广州能源研究所 | A kind of method of storing natural gas hydrate |
| CN111939841A (en) * | 2020-08-13 | 2020-11-17 | 中国科学院西北生态环境资源研究院 | Method for dynamically adjusting water content of medium in hydrate forming process |
| CN114426894A (en) * | 2020-09-29 | 2022-05-03 | 中国石油化工股份有限公司 | Natural gas hydrate phase equilibrium pressure prediction method based on machine learning |
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| CN114426894A (en) * | 2020-09-29 | 2022-05-03 | 中国石油化工股份有限公司 | Natural gas hydrate phase equilibrium pressure prediction method based on machine learning |
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