CN112844275A - Reaction kettle for preparing layered multistage hydrate slurry and preparation method - Google Patents

Reaction kettle for preparing layered multistage hydrate slurry and preparation method Download PDF

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CN112844275A
CN112844275A CN202011225641.9A CN202011225641A CN112844275A CN 112844275 A CN112844275 A CN 112844275A CN 202011225641 A CN202011225641 A CN 202011225641A CN 112844275 A CN112844275 A CN 112844275A
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finished product
hydrate slurry
gas
layered
reaction kettle
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CN112844275B (en
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李占东
干毕成
赵佳彬
李海晨
张海翔
余意
张崇
董钊
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Northeast Petroleum University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18Stationary reactors having moving elements inside
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006Controlling or regulating processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053Details of the reactor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053Details of the reactor
    • B01J19/0066Stirrers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00Feed or outlet devices; Feed or outlet control devices
    • B01J4/001Feed or outlet devices as such, e.g. feeding tubes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00Feed or outlet devices; Feed or outlet control devices
    • B01J4/008Feed or outlet control devices
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00162Controlling or regulating processes controlling the pressure

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Abstract

The invention relates to the field of natural gas hydrate slurry preparation devices, in particular to a reaction kettle for preparing layered multistage hydrate slurry and a preparation method. Through inside the agitator chamber that sets up at reation kettle, synthetic cavity and finished product room, the agitator chamber communicates with synthetic cavity, synthetic cavity and finished product room intercommunication, finished product room and agitator chamber intercommunication, thereby make hydrate thick liquid at the agitator chamber, synthetic cavity and finished product room mesocycle flow, and divide into the multilayer with synthetic cavity through the baffle, every layer switches on each other, and a terminal surface that is close to reation kettle's bottom at the baffle is provided with the gas injection hole, the trachea inserts and cooperatees with the gas injection hole in the baffle, make gas and hydrate thick liquid fully function, make hydrate thick liquid intensive mixing, and set up the further reinforcing of guide plate the mobility of hydrate thick liquid on the baffle, carry to the agitator chamber inside through the hydrate thick liquid that lasts in the finished product room of resistant high-pressure sealed hydraulic turbine simultaneously, thereby the effectual synthetic efficiency that improves hydrate thick liquid.

Description

Reaction kettle for preparing layered multistage hydrate slurry and preparation method
Technical Field
The invention relates to the field of natural gas hydrate slurry preparation devices, in particular to a reaction kettle for preparing layered multistage hydrate slurry and a preparation method.
Background
The hydrate application technology developed aiming at the characteristics of the hydrate is a very active technical field in the research of the hydrate at present. The hydrate slurry mixed transportation technology is regarded as a novel hydrate prevention and control way and an oil gas-water multiphase safe mixed transportation way by the attention of oil gas production and transportation. The cold flow technology, which is widely used at present, allows hydrates to be generated inside the pipes, but ensures that the pipe flow is in a slurry state. The entrained hydrate particles are easy to aggregate and pile up in the flowing process. The normal flow in the pipe is influenced, so that huge loss is caused, and hydrate accumulation and blockage become troublesome problems in production and transportation. The complexity of hydrate accumulation and accumulation is increased by changing the flow field in pipeline transportation due to the bending of the pipeline. At present, the synthesis of hydrate slurries with different volume ratios is only tried, the aggregation and deposition of hydrates in pipelines are avoided, and the problem of blockage in safe transportation is solved. Therefore, it is necessary to study the flow characteristics and deposition law of hydrate slurry under different volume ratios.
Disclosure of Invention
The invention provides a reaction kettle for preparing layered multistage hydrate slurry and a preparation method thereof, which realize the sufficient mixing of the hydrate slurry, so that the hydrate slurry with different volume ratios can be synthesized, the aggregation and the deposition in a pipe can be avoided, and the problem of blockage in safe transportation can be solved.
In order to achieve the purpose, the invention provides the following technical scheme:
a reaction kettle for preparing layered multistage hydrate slurry comprises a reaction kettle arranged in a constant temperature box, a container cavity arranged in the reaction kettle, and a stirrer arranged on the top wall in the container cavity of the reaction kettle, wherein the operation part of the stirrer extends into a stirring chamber right below the stirrer, the stirring chamber is provided with a feed inlet and a discharge outlet, and the discharge outlet is connected with a top feed inlet of a layered multistage synthesis cavity through a pipeline; the bottom discharge port of the layered multi-stage synthesis cavity is connected with the top feed port of the finished product chamber through a pipeline; the bottom discharge port of the finished product chamber is connected to the feed port of the stirring chamber through a pipeline, a three-way valve, a spectrophotometer and a high-pressure-resistant sealed water turbine are sequentially installed on the pipeline from the discharge port of the finished product chamber to the feed port of the stirring chamber, and the sealed water turbine is driven by a motor arranged on the outer wall or the top wall of the stirring chamber; one connecting port of the three-way valve extends out of the reaction kettle and is positioned outside the reaction kettle and used for outputting finished hydrate slurry; and a feed inlet is arranged on the side wall of the layered multistage synthesis cavity close to the top, and the feed inlet is connected with a liquid inlet valve penetrating through the side wall of the reaction kettle through a pipeline, so that external hydrate slurry is conveyed to the inside of the layered multistage synthesis cavity inside the reaction kettle.
Furthermore, n +1 partition plates are arranged in the inner cavity of the layered multi-stage synthesis cavity from top to bottom at equal intervals, and n is greater than or equal to 0; the number of the clapboards is counted from the upper part of the inner cavity downwards in sequence, the clapboards belonging to the odd number are horizontally arranged on the inner part of the same side of the inner cavity, the clapboards belonging to the even number are horizontally arranged on the other side of the inner cavity, the installation sides of the clapboards belonging to the even number are opposite to the installation sides of the clapboard belonging to the odd number, a gap is reserved at one end of the clapboard located at the installation sides of the clapboard belonging to the odd number, one end of the clapboard located at the installation sides of the clapboard belonging to the even number is reserved with a gap, thereby the inner cavity is divided into a plurality of layers through the clapboards, and hydrate slurry in an upper layer space can enter a lower layer.
Still further, each baffle all installs first guide plate on keeping away from the terminal surface of layering multistage synthesis chamber bottom, be an inclined plane on the terminal surface of baffle is kept away from to first guide plate, the inclined plane from the installation side of baffle to leave gapped one end downward sloping to be favorable to the hydrate thick liquid of every layer to flow into in the next layer.
Further, each baffle is inside to be cavity to insert many reposition of redundant personnel trachea that are parallel to each other in the inner space of baffle, many reposition of redundant personnel trachea converge into a mainstream trachea near the one end of baffle installation side, the one end that mainstream trachea is located baffle installation side passes the lateral wall in the multistage synthesis chamber of layering and is connected with the air inlet valve that sets up on the reation kettle lateral wall, the one end that the baffle installation side was kept away from to reposition of redundant personnel trachea is sealed, and be provided with a plurality of gas injection holes in the one end that reposition of redundant personnel trachea is located baffle installation side to the one end of keeping away from the installation side, it is in to correspond also be provided with a plurality of gas injection holes on the baffle is close to the multistage synthesis chamber of layering, and respectively with the gas injection hole one-to-one on the reposition of redundant personnel trachea gas injection hole, and with reposition of redundant personnel trachea gas injection.
Preferably, the diameters of the plurality of gas injection holes on the gas pipe gradually increase from the side close to the installation side of the baffle to the end far from the installation side, and the center distance of each adjacent gas injection hole is 5 CM; the plurality of gas injection holes provided in the gas pipe are set with reference to the following formula, Di+1=γDiWherein gamma is a diffusion coefficient, and gamma is 1.05-2; diIs the diameter of the ith gas injection hole, i is greater than or equal to 1; d1=2~5mm,D1A gas injection hole near the installation side of the clapboard; di+1The diameter of the (i + 1) th gas injection hole.
Preferably, the side walls of the stirring chamber and the finished product chamber are respectively provided with a pressure sensor for detecting the internal pressure of the stirring chamber and the finished product chamber, and probes of the pressure sensors extend into the stirring chamber and the finished product chamber.
Preferably, a pipeline connecting a bottom discharge port of the layered multi-stage synthesis cavity and a top feed port of the finished product chamber extends into the finished product chamber, and a diffuser is arranged on the end of the pipeline extending into the finished product chamber; the pipeline connecting the discharge port of the stirring chamber and the feed inlet at the top of the layered multi-stage synthesis cavity extends into the layered multi-stage synthesis cavity, and a diffuser is arranged at the end position where the pipeline extends into the layered multi-stage synthesis cavity.
Preferably, the second guide plate is installed to the finished product room bottom, and a terminal surface that the finished product room bottom was kept away from to the second guide plate is the inclined plane, and the one end that the inclined plane is close to the finished product room discharge gate is less than the distance that finished product room discharge gate one end was kept away from the finished product room bottom surface to the inclined plane apart from the distance of finished product room bottom surface, from the hydrate slurry of being convenient for flow to the one end that is close to the finished product room discharge gate by oneself.
The preparation method of the layered multistage hydrate slurry adopts the reaction kettle, and comprises the following specific steps:
step 1: starting the constant temperature box, adjusting the temperature of the constant temperature box to be within the temperature range of 260-272K, starting a motor in the original layered multi-stage hydrate slurry preparation system through a control terminal of the original layered multi-stage hydrate slurry preparation system, enabling a liquid source to enter a layered multi-stage synthesis cavity from a liquid inlet valve, and then entering a finished product chamber through the layered multi-stage synthesis cavity; starting the motor, driving the high-pressure sealing water turbine by the motor, starting the stirrer simultaneously, and conveying the liquid source in the finished product chamber to the stirring chamber by the high-pressure sealing water turbine, so that the liquid source continuously and circularly flows in the stirring chamber, the layered multi-stage synthesis cavity and the finished product chamber, opening the air inlet valve, introducing an air source, injecting air into the layered multi-stage synthesis cavity through the air injection hole after the air enters from the air inlet valve, and fully acting the air and the liquid to uniformly flow in a film shape along the inner wall of the layered multi-stage synthesis cavity under the action of temperature and pressure;
step 2: keeping the temperature of the constant temperature box between 260 ℃ and 272K, and the pressure in the reaction kettle is 2-8 Mpa; waiting for T minutes after gas injection, opening a spectrophotometer to sample the hydrate slurry, and executing the step 3 on the hydrate slurry reaching the specified volume fraction; continuously preparing the hydrate slurry which does not reach the specified volume fraction, namely starting a high-pressure-resistant sealed water turbine and a stirrer, continuously enabling the hydrate slurry to circularly flow in a stirring chamber, a layered multistage synthesis cavity and a finished product chamber, enabling gas to enter a diversion gas pipe from a gas inlet valve, injecting the gas into the layered multistage synthesis cavity through the diversion gas pipe, enabling the gas and the hydrate slurry to fully act, and executing the step 3 until the hydrate slurry sampled and detected by a spectrophotometric detector reaches the specified volume fraction;
and step 3: opening a valve from the reaction kettle to the constant-pressure storage tank, and then opening a three-way valve from a finished product chamber to a pipeline of the high-pressure-resistant sealed water turbine; and (4) guiding the hydrate slurry in the finished product chamber to a constant pressure box of the original layered multistage hydrate slurry preparation system.
Preferably, the gas injection amount in the step 2 is based on the gas injection amount calculated by the following formula,
Figure RE-RE-GDA0003010767110000041
the V isiThe volume amount of gas injected for the ith time; vi+1The volume amount of gas injected for the (i + 1) th time; v is the total volume of the gas to be injected; alpha is a gas grading coefficient, and alpha is 2-7; beta is a gas correction coefficient, and beta is 1.00-1.05; the setting of the specific time T should satisfy the result calculated by the following formula,
Figure RE-RE-GDA0003010767110000042
wherein T isiFor the ith time interval, T1=30~60min;Ti+1Is the (i + 1) th time interval; alpha is the gas classification coefficient.
Compared with the prior art, the invention has the beneficial effects that: the hydrate slurry is fully mixed in the reaction kettle, the aggregation and deposition of the hydrate in the pipeline are avoided, and the problem of blockage in safe transportation is solved. And further the mobility of hydrate thick liquid has been strengthened through setting up the guide plate, and the hydrate thick liquid in the last finished product room of continuous will be carried to the stirring indoor portion through the sealed hydraulic turbine of nai high pressure simultaneously to the effectual synthetic efficiency who improves hydrate thick liquid.
Drawings
FIG. 1 is a schematic view of the overall structure of a reaction vessel according to the present invention;
FIG. 2 is a schematic view of the end of the baffle plate of the present invention near the bottom of the reaction vessel;
FIG. 3 is a detail view of the splitter and mainstream gas ducts of the present invention;
FIG. 4 is a schematic view of the installation position of the bypass air tube of the present invention;
description of reference numerals: 1. a reaction kettle; 2. a stirrer; 3. a stirring chamber; 4. a layered and multistage synthesis cavity; 5. a finished product room; 6. a three-way valve; 7. a spectrophotometer; 8. a liquid inlet valve; 9. an electric motor; 10. a high pressure resistant sealed water turbine; a separator plate; 12. an intake valve; 13. a baffle; 14. a diffuser; 15. a pressure sensor; 16. a gas distributing pipe; 17. a main air flow pipe.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A reaction kettle for preparing layered multistage hydrate slurry comprises a reaction kettle 1 arranged in a constant temperature box, a container cavity arranged in the reaction kettle 1, and a stirrer 2 arranged on the top wall in the container cavity of the reaction kettle 1, wherein the operation part of the stirrer 2 extends into a stirring chamber 3 right below the stirrer 2, the stirring chamber 3 is provided with a feed inlet and a discharge outlet, and the discharge outlet is connected with a top feed inlet of a layered multistage synthesis cavity 4 through a pipeline; the bottom discharge ports of the layered multi-stage synthesis cavities 4 are connected into the top feed port of the sample chamber 5 through a pipeline; a discharge port at the bottom of the finished product chamber 5 is connected to a feed port of the stirring chamber 3 through a pipeline, a three-way valve 6, a spectrophotometer 7 and a high-pressure-resistant sealing water turbine 10 are sequentially installed on the pipeline from the discharge port of the finished product chamber 5 to the feed port of the stirring chamber 3, and the sealing water turbine is driven by a motor 9 arranged on the outer wall or the top wall of the stirring chamber 3; one connecting port of the three-way valve 6 extends out of the reaction kettle 1 and is positioned outside the reaction kettle 1 and used for outputting finished hydrate slurry; and a feed inlet is arranged on the side wall of the layered multistage synthesis cavity 4 close to the top, and the feed inlet is connected with a liquid inlet valve 8 penetrating through the side wall of the reaction kettle 1 through a pipeline, so that external hydrate slurry is conveyed to the inside of the layered multistage synthesis cavity 4 inside the reaction kettle 1.
Further, n +1 partition plates 11 are arranged in the inner chamber of the layered multi-stage synthesis cavity 4 from top to bottom at equal intervals, wherein n is greater than or equal to 0; the number of the partition boards 11 is counted from the upper part of the inner cavity downwards in sequence, the partition boards 11 belonging to the odd number are horizontally arranged on the inner part of the same side of the inner cavity, the partition boards 11 belonging to the even number are horizontally arranged on the other side of the inner cavity, the installation sides of the even number partition boards 11 are opposite to the installation sides of the odd number partition boards 11, one ends of the odd number partition boards 11, which are positioned on the installation sides of the even number partition boards 11, are provided with gaps, one ends of the even number partition boards 11, which are positioned on the installation sides of the odd number partition boards 11, are provided with gaps, so that the inner cavity is divided into a plurality of layers through the partition boards 11, and hydrate slurry in an upper layer space can enter.
Still further, each baffle 11 is far away from and all installs first guide plate 13 on the terminal surface of layering multistage synthesis chamber 4 bottom, first guide plate 13 is a slope on keeping away from the terminal surface of baffle 11, and the slope is from the installation side of baffle 11 to keeping gapped one end downward sloping to be favorable to the hydrate thick liquid of every layer to flow into in the next layer.
Furthermore, the interior of each partition plate 11 is hollow, a plurality of parallel branch air pipes 16 are inserted into the interior space of the partition plate 11, the ends of the plurality of branch air pipes 16 close to the installation side of the partition plate 11 are converged into a main air pipe 17, one end of the main air pipe 17 located at the installation side of the partition plate 11 penetrates through the side wall of the layered multistage synthesis cavity 4 to be connected with an air inlet valve 12 arranged on the side wall of the reaction kettle 1, one end of the branch air pipe 16 far away from the installation side of the partition plate 11 is closed, and a plurality of gas injection holes are provided from the end of the divided gas pipe 16 on the installation side of the partition 11 to the end remote from the installation side, a plurality of gas injection holes are correspondingly arranged on one end surface of the clapboard 11 close to the layered multi-stage synthesis cavity 4, and respectively correspond to the gas injection holes on the branch gas pipe 16 one-to-one, and are the same as the arrangement of the gas injection holes of the branch gas pipe 16 and the diameters of the corresponding gas injection holes.
Preferably, the diameters of the plurality of gas injection holes on the gas pipe gradually increase from the side close to the installation of the baffle plate 11 to the end far from the installation side, and the center-to-center distance of each adjacent gas injection hole is 5 CM; arranged on said tracheaThe plurality of gas injection holes are arranged with reference to the following formula, Di+1=γDiWherein gamma is a diffusion coefficient, and gamma is 1.05-2; diIs the diameter of the ith gas injection hole, i is greater than or equal to 1; d1=2~5mm,D1A gas injection hole near the installation side of the diaphragm 11; di+1The diameter of the (i + 1) th gas injection hole.
Preferably, the side walls of the stirring chamber 3 and the product chamber 5 are both provided with a pressure sensor 15 for detecting the internal pressure of the stirring chamber 3 and the product chamber 5, and the probes of the pressure sensor 15 extend into the stirring chamber 3 and the product chamber 5.
Preferably, a pipeline connecting a bottom discharge port of the layered multi-stage synthesis cavity 4 and a top feed port of the finished product chamber 5 extends into the finished product chamber 5, and a diffuser 14 is arranged at the end of the pipeline extending into the finished product chamber 5; the pipeline connecting the discharge hole of the stirring chamber 3 and the feed inlet at the top of the layered multi-stage synthesis cavity 4 extends into the layered multi-stage synthesis cavity 4, and a diffuser 14 is arranged at the end position where the pipeline extends into the layered multi-stage synthesis cavity 4.
Preferably, second guide plate 13 is installed to finished product room 5 bottom, and a terminal surface that finished product room 5 bottoms was kept away from to second guide plate 13 is the inclined plane, and the distance that the one end that the inclined plane is close to finished product room 5 discharge gate is less than the inclined plane and keeps away from the distance of finished product room 5 discharge gate one end apart from finished product room 5 bottom surface, from the hydrate slurry of being convenient for flow to the one end that is close to finished product room 5 discharge gate by oneself.
The preparation method of the layered multistage hydrate slurry adopts the reaction kettle 1, and comprises the following specific steps:
step 1: starting the constant temperature box, adjusting the temperature of the constant temperature box to be within the temperature range of 260-272K, starting a motor in the original layered multi-stage hydrate slurry preparation system through a control terminal of the original layered multi-stage hydrate slurry preparation system, enabling a liquid source to enter a layered multi-stage synthesis cavity 4 from a liquid inlet valve 8, and then entering a finished product chamber 5 through the layered multi-stage synthesis cavity 4; meanwhile, the motor 9 is started, the high-pressure sealing water turbine is driven by the motor 9, the stirrer 2 is started, the high-pressure sealing water turbine 10 conveys the liquid source in the finished product chamber 5 to the stirring chamber 3, so that the liquid source continuously and circularly flows in the stirring chamber 3, the layered multi-stage synthesis chamber 4 and the finished product chamber 5, the air inlet valve 12 is opened, the air source is introduced, the air enters from the air inlet valve 12 and then is injected into the layered multi-stage synthesis chamber 4 through the air injection hole, and the air and the liquid fully act to uniformly flow in a film shape along the inner wall of the layered multi-stage synthesis chamber 4 under the action of temperature and pressure;
step 2: keeping the temperature of the constant temperature box between 260 ℃ and 272K, and the pressure in the reaction kettle 1 is 2-8 Mpa; waiting for T minutes after gas injection, starting a spectrophotometer 7 to sample the hydrate slurry, and executing the step 3 on the hydrate slurry reaching the specified volume fraction; continuously preparing the hydrate slurry which does not reach the designated volume fraction, namely starting the high-pressure-resistant sealed water turbine 10 and the stirrer 2, continuously enabling the hydrate slurry to circularly flow in the stirring chamber 3, the layered multistage synthesis cavity 4 and the finished product chamber 5, enabling gas to enter the gas distribution pipe 16 from the gas inlet valve 12, injecting the gas into the layered multistage synthesis cavity 4 through the gas distribution pipe 16, enabling the gas and the hydrate slurry to fully act, and executing the step 3 after the hydrate slurry sampled and detected by the spectrophotometric detector reaches the designated volume fraction;
and step 3: after a valve from the reaction kettle 1 to the constant-pressure storage tank is opened, a three-way valve 6 from a finished product chamber 5 to a pipeline of a high-pressure-resistant sealed water turbine 10 is opened; and (3) guiding the hydrate slurry in the finished product chamber 5 to a constant pressure box of the original layered multistage hydrate slurry preparation system.
Preferably, the gas injection amount in the step 2 is based on the gas injection amount calculated by the following formula,
Figure RE-RE-GDA0003010767110000081
the V isiThe volume amount of gas injected for the ith time; vi+1The volume amount of gas injected for the (i + 1) th time; v is the total volume of the gas to be injected; alpha is a gas grading coefficient, and alpha is 2-7; beta is a gas correction coefficient, and beta is 1.00-1.05; the setting of the specific time T should satisfy the result calculated by the following formula,
Figure RE-RE-GDA0003010767110000082
wherein T isiFor the ith time interval, T1=30~60min;Ti+1Is the (i + 1) th time interval;alpha is the gas classification coefficient.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.

Claims (10)

1. A reation kettle for preparation of multistage hydrate thick liquid of layering which characterized in that: the device comprises a reaction kettle (1) arranged in a constant temperature box, a container cavity arranged in the reaction kettle (1), and a stirrer (2) arranged on the top wall in the container cavity of the reaction kettle (1), wherein the operation part of the stirrer (2) extends into a stirring chamber (3) right below the stirrer (2), a feeding hole and a discharging hole are arranged on the stirring chamber (3), and the discharging hole is connected with a top feeding hole of a layered multi-stage synthesis cavity (4) through a pipeline; the bottom discharge hole of the layered multi-stage synthesis cavity (4) is connected with the top feed inlet of the finished product chamber (5) through a pipeline; the bottom discharge port of the finished product chamber (5) is connected to the feed port of the stirring chamber (3) through a pipeline, a three-way valve (6), a spectrophotometer (7) and a high-pressure-resistant sealing water turbine (10) are sequentially installed on the pipeline from the discharge port of the finished product chamber (5) to the feed port of the stirring chamber (3), and the high-pressure-resistant sealing water turbine (9) is driven by a motor (9) arranged on the outer wall or the top wall of the stirring chamber (3); one connecting port of the three-way valve (6) extends out of the reaction kettle (1) and is positioned outside the reaction kettle (1) and used for outputting finished hydrate slurry; and a feed inlet is arranged on the side wall of the layered multi-stage synthesis cavity (4) close to the top, and the feed inlet is connected with a liquid inlet valve (8) penetrating through the side wall of the reaction kettle (1) through a pipeline.
2. The reaction kettle for layered multistage hydrate slurry preparation according to claim 1, wherein: n +1 partition plates (11) are arranged in the inner cavity of the layered multi-stage synthesis cavity (4) from top to bottom at equal intervals, and n is greater than or equal to 0; the number of the partition boards (11) is counted from the upper part of the inner cavity downwards in sequence, the partition boards (11) belonging to the singular number are horizontally arranged on the inner part of the same side of the inner cavity, the partition boards (11) belonging to the even number are horizontally arranged on the other side of the inner cavity, the installation sides of the partition boards (11) belonging to the odd number are opposite to the installation sides of the partition boards (11) belonging to the singular number, gaps are reserved at one ends of the partition boards (11) belonging to the odd number, the partition boards (11) are arranged at one ends of the installation sides of the partition boards (11) belonging to the even number, the inner cavity is divided into a plurality of layers through the partition boards (11), and hydrate slurry in an upper layer space can enter a lower layer space through the gaps to form an S-shaped hydrate slurry flowing line.
3. The reaction kettle for layered multistage hydrate slurry preparation according to claim 2, wherein: every all install first guide plate (13) on baffle (11) keep away from the terminal surface of layering multistage synthetic chamber (4) bottom, be an inclined plane on first guide plate (13) keep away from a terminal surface of baffle (11), the installation side of baffle (11) is followed to the inclined plane and is left gapped one end downward sloping.
4. The reaction kettle for layered multistage hydrate slurry preparation according to claim 2, wherein: each partition plate (11) is hollow, a plurality of parallel branch air pipes (16) are inserted into the inner space of each partition plate (11), the branch air pipes (16) are converged into a main air pipe (17) at one end close to the installation side of each partition plate (11), one end of each main air pipe (17) at the installation side of each partition plate (11) penetrates through the side wall of the corresponding layered multi-stage synthesis cavity (4) to be connected with an air inlet valve (12) arranged on the side wall of the reaction kettle (1), one end, far away from the installation side of each partition plate (11), of each branch air pipe (16) is closed, a plurality of air injection holes are formed in one end, far away from the installation side, of each branch air pipe (16) at one end of the installation side of each partition plate (11), a plurality of air injection holes are correspondingly formed in one end face, close to the corresponding layered multi-stage synthesis cavity (4), of each partition plate (11), and the air injection holes on the branch air, and the arrangement of the gas injection holes of the gas distribution pipe (16) and the corresponding gas injection hole diameter are the same.
5. The reaction kettle for layered multistage hydrate slurry preparation according to claim 4, wherein: the diameters of a plurality of gas injection holes on the gas pipe are gradually increased from the mounting side close to the clapboard (11) to one end far away from the mounting side, and the center distance of each adjacent gas injection hole is 5 CM; the plurality of gas injection holes provided in the gas pipe are set with reference to the following formula, Di+1=γDiWherein gamma is a diffusion coefficient, and gamma is 1.05-2; diIs the diameter of the ith gas injection hole, i is greater than or equal to 1; d1=2~5mm,D1A gas injection hole near the installation side of the clapboard (11); di+1The diameter of the (i + 1) th gas injection hole.
6. The reaction kettle for layered multistage hydrate slurry preparation according to claim 1, wherein: stirring room (3) and finished product room (5) lateral wall all install and are used for detecting pressure sensor (15) of stirring room (3) and finished product room (5) internal pressure, and pressure sensor's (15) probe stretches into inside stirring room (3) and finished product room (5).
7. The reaction kettle for layered multistage hydrate slurry preparation according to claim 1, wherein: a pipeline connecting a bottom discharge hole of the layered multi-stage synthesis cavity (4) and a top feed hole of the finished product chamber (5) extends into the finished product chamber (5), and a diffuser (14) is arranged at the end of the pipeline extending into the finished product chamber (5); the pipeline connecting the discharge port of the stirring chamber (3) and the feed inlet at the top of the layered multi-stage synthesis cavity (4) extends into the layered multi-stage synthesis cavity (4), and a diffuser (14) is arranged at the end position where the pipeline extends into the layered multi-stage synthesis cavity (4).
8. The reaction kettle for layered multistage hydrate slurry preparation according to claim 1, wherein: second guide plate (13) are installed to finished product room (5) bottom, and a terminal surface that finished product room (5) bottom was kept away from in second guide plate (13) is the inclined plane, and the distance that finished product room (5) discharge gate one end was kept away from finished product room (5) bottom surface to the inclined plane is less than the distance that finished product room (5) discharge gate one end was kept away from finished product room (5) bottom surface to the inclined plane.
9. A preparation method of layered multistage hydrate slurry is characterized by comprising the following steps: the method comprises the following steps:
step 1: starting the constant temperature box, adjusting the temperature of the constant temperature box to be within the temperature range of 260-272K, starting a motor in the original layered multi-stage hydrate slurry preparation system through a control terminal of the original layered multi-stage hydrate slurry preparation system, enabling a liquid source to enter a layered multi-stage synthesis cavity (4) from a liquid inlet valve (8), and then entering a finished product chamber (5) through the layered multi-stage synthesis cavity (4); meanwhile, a motor (9) is started, a high-pressure sealing water turbine is driven by the motor (9), a stirrer (2) is started, a high-pressure sealing water turbine (10) conveys a liquid source in a finished product chamber (5) to the stirring chamber (3), so that the liquid source continuously and circularly flows in the stirring chamber (3), the layered multi-stage synthesis chamber (4) and the finished product chamber (5), an air inlet valve (12) is opened, an air source is introduced, air enters from the air inlet valve (12) and then is injected into the layered multi-stage synthesis chamber (4) through an air injection hole, and under the action of temperature and pressure, the air and the liquid fully act to uniformly flow in a film shape along the inner wall of the layered multi-stage synthesis chamber (4);
step 2: the temperature of the constant temperature box is kept between 260 ℃ and 272K, and the pressure in the reaction kettle (1) is 2-8 Mpa; waiting for T minutes after gas injection, opening a spectrophotometer (7) to sample the hydrate slurry, and executing the step 3 on the hydrate slurry reaching the specified volume fraction; continuously preparing the hydrate slurry which does not reach the designated volume fraction, namely starting a high-pressure-resistant sealed water turbine (10) and a stirrer (2), continuously enabling the hydrate slurry to circularly flow in a stirring chamber (3), a layered multi-stage synthesis cavity (4) and a finished product chamber (5), enabling gas to enter a gas distribution pipe (16) from a gas inlet valve (12), injecting the gas into the layered multi-stage synthesis cavity (4) through the gas distribution pipe (16), enabling the gas and the hydrate slurry to fully act, and executing the step (3) until the hydrate slurry sampled and detected by a spectrophotometric detector reaches the designated volume fraction;
and step 3: after a valve from the reaction kettle (1) to a constant-pressure storage tank is opened, a three-way valve (6) from a finished product chamber (5) to a pipeline of a high-pressure-resistant sealed water turbine (10) is opened; and (3) guiding the hydrate slurry in the finished product chamber (5) to a constant pressure box of the original layered multistage hydrate slurry preparation system.
10. The method for preparing a layered multistage hydrate slurry according to claim 9, wherein: the gas injection amount in the step 2 is based on the gas injection amount calculated by the following formula,
Figure FDA0002763569050000041
Figure FDA0002763569050000042
Vi+1=0.1αVi(ii) a The V isiThe volume amount of gas injected for the ith time; vi+1The volume amount of gas injected for the (i + 1) th time; v is the total volume of the gas to be injected; alpha is a gas grading coefficient, and alpha is 2-7; beta is a gas correction coefficient, and beta is 1.00-1.05; the setting of the specific time T should satisfy the result calculated by the following formula,
Figure FDA0002763569050000043
wherein T isiFor the ith time interval, T1=30~60min;Ti+1Is the (i + 1) th time interval; alpha is the gas classification coefficient.
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