CN108160003A - A kind of quick equipment for continuously preparing gas hydrate - Google Patents

A kind of quick equipment for continuously preparing gas hydrate Download PDF

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Publication number
CN108160003A
CN108160003A CN201711297879.0A CN201711297879A CN108160003A CN 108160003 A CN108160003 A CN 108160003A CN 201711297879 A CN201711297879 A CN 201711297879A CN 108160003 A CN108160003 A CN 108160003A
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CN
China
Prior art keywords
ice
reaction kettle
unit
hydrate
temperature
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CN201711297879.0A
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Chinese (zh)
Inventor
史伶俐
梁德青
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Guangzhou Institute of Energy Conversion of CAS
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Guangzhou Institute of Energy Conversion of CAS
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Priority to CN201711297879.0A priority Critical patent/CN108160003A/en
Publication of CN108160003A publication Critical patent/CN108160003A/en
Pending legal-status Critical Current

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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
    • B01J3/00Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/04Pressure vessels, e.g. autoclaves
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/002Component parts of these vessels not mentioned in B01J3/004, B01J3/006, B01J3/02 - B01J3/08; Measures taken in conjunction with the process to be carried out, e.g. safety measures
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/02Feed or outlet devices therefor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2203/00Processes utilising sub- or super atmospheric pressure
    • B01J2203/06High pressure synthesis
    • B01J2203/0675Structural or physico-chemical features of the materials processed
    • B01J2203/068Crystal growth

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses a kind of quick equipment for continuously preparing gas hydrate, the air supply unit for be equipped with the reaction kettle of water leg including outside, air source being provided for the reaction kettle, ice liquid is provided for the reaction kettle unit and data acquisition process unit for acquiring and recording the temperature of reaction kettle and pressure is collected by filtration for ice liquid unit, for controlling the temperature control unit of the additional sleeving temperature, connecting with the reaction kettle and being used to generating it hydrate that hydrate crystal is filtered and collects;The rear end that unit is collected by filtration in the hydrate is connect by quick-connecting valve with described for ice liquid unit.The present invention solves the defects of incomplete hydrate formation in Conventional Hydrate generating means, mechanical agitation slurry or magneton internal residual, reaction process is discontinuous;It is experimental provision simple economy, easy to operate;Complete and uniform gas hydrate can be generated, improves the efficiency of gas storage and transportation.

Description

A kind of quick equipment for continuously preparing gas hydrate
Technical field
A kind of quickly prepare the present invention relates to the experimental facilities for preparing gas hydrate more particularly to continuously gas hydrate Equipment.
Background technology
Gas hydrate is in low temperature height by gas molecule (such as methane, carbon dioxide, nitrogen, hydrogen sulfide) and hydrone The cage modle crystalline compounds of a type ice-like generated under the conditions of pressure.In recent years, go deep into gas hydrate research, find A kind of new and effective industrial technology can be become by carrying out gas separation and storage and transportation using gas hydrate.
Under study for action, shadow of the stirring to the generation theorem property, particularly induction time and gas-storing capacity of hydrate is found Sound is very big.Current existing stirring technique is internal mechanical stirring or magnetic agitation.During stirring, reaction vessel interior is placed with Mechanical agitation is starched or magneton.All there are shortcomings for both modes:First, the generation caking of gas-water interface hydrate can hinder lower part Hydrate continues to generate, and the hydrate block consolidation that mechanical agitation slurry or magneton can be also generated can not be completed to be stirred and be appointed Business;Second is that in the transportational process after hydrate generates, mechanical agitation slurry or magneton are connected with hydrate, can not take out; Third, hydrate can not carry out continuous production.
Invention content
The purpose of the present invention is overcoming above-mentioned the deficiencies in the prior art, provide and a kind of quickly continuously prepare gas hydrate Equipment, the device systems are simple and convenient to operate, and the substantially uniformity applied to gas hydrate generates.
The present invention is achieved through the following technical solutions:A kind of quick equipment for continuously preparing gas hydrate, packet Outside is included to be equipped with the reaction kettle of water leg, the air supply unit that air source is provided for the reaction kettle, provide ice liquid for the reaction kettle For ice liquid unit, for controlling the temperature control unit of the additional sleeving temperature, connect with the reaction kettle and be used for it Unit is collected by filtration and for acquiring and recording the reaction kettle in the hydrate that generation hydrate crystal is filtered and collects The data acquisition process unit of temperature and pressure;The rear end that unit is collected by filtration in the hydrate passes through quick-connecting valve and the confession Ice liquid unit connects.
Reaction kettle is the container of air water system reaction generation hydrate, and the setting of water leg can make temperature control unit Control system temperature;It is the device for carrying out separation of solid and liquid that unit, which is collected by filtration, in hydrate;Data acquisition process unit can be remembered automatically Temperature, the pressure in reaction kettle are recorded, the hydrate convenient for system in analysis reaction kettle generates progress.
The air supply unit includes gas cylinder tank, constant pressure intake valve, gas unidirectional strainer valve, bubbling nozzle and admission line; The side of the reaction kettle is provided with air inlet, and top is provided with exhaust outlet;The gas outlet of the gas cylinder tank by it is described into Gas pipeline is sequentially connected the constant pressure intake valve, the air inlet and the bubbling nozzle, and the bubbling nozzle is located at described The bottom of reaction kettle;The exhaust outlet by the admission line connect access after the gas unidirectional strainer valve be located at it is described into On admission line between gas port and the constant pressure intake valve.Gas cylinder tank, constant pressure intake valve and bubbling nozzle form induction pathway, Realization supplies reaction kettle;Gas unidirectional strainer valve forms the gas return path of unreacting gas, helps to improve gas Effective rate of utilization;Gas can be disperseed and uniformly sprayed by bubbling nozzle, be conducive to homogeneous reaction.
The ultrasonic wave trash ice for including ice flow container for ice liquid unit, the ice liquid in the ice flow container being broken into ice slurry Device, ice flow container valve, ice liquid pump, ice liquid inlet valve and return line;The liquid outlet of the ice flow container is sequentially connected with by outlet tube It is accessed in the reaction kettle after ice flow container valve, ice liquid pump, ice liquid inlet valve.
All multi-layer filtrating equipments inside unit are collected by filtration in the hydrate;The opposite side of the reaction kettle by connecing soon Head is collected by filtration unit with the hydrate and connect, and the rear end that unit is collected by filtration in the hydrate is connected by the return line The ice flow container is accessed after connecing the quick-connecting valve.
The data acquisition process unit includes data acquisition processing device and computer data processing system;The data Acquisition processing device includes temperature sensor, pressure sensor and data acquisition control card;Be provided at the top of the reaction kettle with The temperature and pressure mouth that the temperature sensor, pressure sensor connect, the temperature sensor, pressure sensor are respectively connected to the number According to acquisition and control card, the data acquisition control card connects with the computer data processing system.Temperature sensor, pressure pass Sensor is by data acquisition control card, temperature, pressure in limnograph reaction kettle, convenient for system in analysis reaction kettle Hydrate generation progress.
The reaction kettle uses autoclave.
The multi-layer filtrating equipment is using the vertically arranged filter screen of multilayer.The vertically arranged filter screen multilayer of multilayer is erected To the filter screen of setting, the hydrate crystal of generation can be filtered and be collected.
The temperature control unit is constant temperature water bath.
It is compared with the prior art, the advantage of the invention is that:
(1) complete and uniform gas hydrate can be generated, improves the efficiency of gas storage and transportation;
(2) there is no the residual of mechanical agitation slurry or magneton in reaction vessel, system can both be strengthened passing with continuous operation Hot mass transfer effect, and reaction process can be controlled to realize hydrate generation or flow collection, facilitate and carry out next step transport operation.
Description of the drawings
Fig. 1 is the experimental facilities schematic diagram of the embodiment of the present invention.
Reference numeral meaning in figure:1st, gas cylinder tank;2nd, constant pressure intake valve;3rd, gas unidirectional strainer valve;4th, at data acquisition Manage device;5th, computer data processing system;6th, kettle is collected by filtration in hydrate;7th, reaction kettle;8th, ice liquid inlet valve;9th, thermostatted water Bath;10th, ice liquid pump;11st, ice flow container valve;12nd, ice flow container;13rd, ultrasonic wave ice breaker and chipper;14th, fast joint;15th, quick-connecting valve; 16th, bubbling nozzle.
Specific embodiment
Present disclosure is described in further details with reference to the accompanying drawings and detailed description.
Embodiment
Refering to Fig. 1, for a kind of quick equipment for continuously preparing gas hydrate, the reaction kettle of water leg is equipped with including outside 7th, be reaction kettle 7 provide the air supply unit of air source, be reaction kettle 7 provide ice liquid for ice liquid unit, for controlling outer jacketed temperature The temperature control unit of degree connects with reaction kettle 7 and for generating the hydrate that hydrate crystal is filtered and collects to it Unit and the data acquisition process unit for acquiring and recording 7 temperature and pressure of reaction kettle is collected by filtration;Hydrate filters The rear end of collector unit is connect by quick-connecting valve 15 with for ice liquid unit.
Reaction kettle 7 is the container of air water system reaction generation hydrate, and the setting of water leg can make temperature control unit Control system temperature;It is the device for carrying out separation of solid and liquid that unit, which is collected by filtration, in hydrate;Data acquisition process unit can be remembered automatically Temperature, the pressure in reaction kettle 7 are recorded, the hydrate convenient for system in analysis reaction kettle 7 generates progress.
Air supply unit includes gas cylinder tank 1, constant pressure intake valve 2, gas unidirectional strainer valve 3, bubbling nozzle 16 and admission line; The side of reaction kettle 7 is provided with air inlet, and top is provided with exhaust outlet;The gas outlet of gas cylinder tank 1 by admission line successively Connection constant pressure intake valve 2, air inlet and bubbling nozzle 16, bubbling nozzle 16 are located at the bottom of reaction kettle 7;Exhaust outlet by into Access is on the admission line between air inlet and constant pressure intake valve 2 after gas pipeline connection gas unidirectional strainer valve 3.Gas cylinder tank 1st, constant pressure intake valve 2 forms induction pathway with bubbling nozzle 16, realizes and reaction kettle 7 is supplied;3 structure of gas unidirectional strainer valve Into the gas return path of unreacting gas, the effective rate of utilization of gas is helped to improve;Bubbling nozzle 16 can disperse gas simultaneously It uniformly sprays, is conducive to homogeneous reaction.
For ice liquid unit include ice flow container 12, the ultrasonic wave ice breaker and chipper 13 that the ice liquid in ice flow container 12 is broken into ice slurry, Ice flow container valve 11, ice liquid pump 10, ice liquid inlet valve 8 and return line;The liquid outlet of ice flow container 12 is sequentially connected with by outlet tube It is accessed in reaction kettle 7 after ice flow container valve 11, ice liquid pump 10, ice liquid inlet valve 8.
All multi-layer filtrating equipments inside unit are collected by filtration in hydrate;The opposite side of reaction kettle 7 by fast joint 14 with Unit connection is collected by filtration in hydrate, and the rear end that unit is collected by filtration in hydrate is followed by by return line connection quick-connecting valve 15 Enter ice flow container 12.
Data acquisition process unit includes data acquisition processing device 4 and computer data processing system 5;At data acquisition It manages device 4 and includes temperature sensor, pressure sensor and data acquisition control card;7 top of reaction kettle is provided with and temperature sensing The temperature and pressure mouth that device, pressure sensor connect, temperature sensor, pressure sensor are respectively connected to data acquisition control card, and data are adopted Collection control card connects with computer data processing system 5.Temperature sensor, pressure sensor by data acquisition control card, from The dynamic temperature measured in record reaction kettle 7, pressure, the hydrate convenient for system in analysis reaction kettle 7 generate progress.
Reaction kettle 7 uses autoclave 7.Autoclave 7 (magnetic force autoclave 7) is magnetic drive device application In typical case's innovation of consersion unit, the shaft sealing leakage that it fundamentally solves former packing seal, mechanical seal can not overcome Problem is the ideal device of the domestic chemical reaction carried out at present under high temperature, high pressure, especially without any leakage and pollution It is to carry out inflammable, explosive, poisonous medium chemical reaction, more shows its superiority.
Multi-layer filtrating equipment is using the vertically arranged filter screen of multilayer.The vertically arranged filter screen multilayer of multilayer is vertically set The hydrate crystal of generation can be filtered and collected by the filter screen put.
Temperature control unit is constant temperature water bath 9.Water can be controlled by controlling the temperature of liquid in constant temperature water bath 9 The temperature of 7 external jacket of object reaction kettle is closed, and then controls the temperature of system in reaction kettle 7, temperature control precision is ± 0.1K.
Water leg in the present embodiment, it is gas generator important component, and general gas generator body is designed to Water leg form, some are also referred to as water leg boiler, and the purpose is to prevent the slag of coal or ash in gasification from attaching shaft, shadow Ring the uniform decline of the bed of material.
The quick process for continuously preparing gas hydrate includes the following steps in this embodiment:
(1) start constant temperature water bath 9, autoclave 7 is cooled to set temperature;
(2) ultrasonic wave ice breaker and chipper 13 is opened, the ice liquid in ice flow container 12 is broken into ice slurry;
(3) ice flow container valve 11, ice liquid pump 10 and ice liquid inlet valve 8 are opened, ice to be reacted will be poured in autoclave 7 Slurry;
(4) constant pressure intake valve 2 is opened, reaction gas into autoclave 7 is filled in the form of bubbling by bubbling nozzle 16 Body, generates gas hydrate, and unreacting gas forms gas return path by gas unidirectional strainer valve 3;
(5) it after data acquisition processing device 4 and the operation of computer data processing system 5 reach homeostasis, repeats to walk Suddenly (3), make generation complete hydrate autoclave 7 is discharged under the action of ice liquid, hydrate be collected by filtration in kettle 6 into Row separation obtains the hydrate crystal of generation, and unreacted ice slurry is made by being recycled in ice slurry circuit feeding ice flow container 12 With;
(6) after the hydrate that hydrate is collected by filtration in kettle 6 reaches rated capacity, fast joint 14 is opened, is more renewed Kettle 6 is collected by filtration in hydrate, and realization continuously prepares gas hydrate;
(7) it generates complete hydrate kettle 6 is collected by filtration and hydrate crystal block is prepared under liquid nitrogen booster action, into follow-up Storage and transportation step.
Above-listed detailed description is illustrating for possible embodiments of the present invention, which is not to limit this hair Bright the scope of the claims, all equivalence enforcements or change without departing from carried out by the present invention are intended to be limited solely by the scope of the claims of this case.

Claims (8)

1. a kind of quick equipment for continuously preparing gas hydrate, it is characterised in that:The reaction kettle of water leg is equipped with including outside (7), be the reaction kettle (7) provide air source air supply unit, be the reaction kettle (7) offer ice liquid for ice liquid unit, In control the temperature control unit of the additional sleeving temperature, connect with the reaction kettle (7) and for generating hydrate to it is brilliant The hydrate that body is filtered and collects is collected by filtration unit and for acquiring and recording the reaction kettle (7) temperature and pressure The data acquisition process unit of power;The rear end that unit is collected by filtration in the hydrate supplies ice liquid by quick-connecting valve (15) with described Unit connects.
2. the quick equipment for continuously preparing gas hydrate according to claim 1, it is characterised in that:The air supply unit Including gas cylinder tank (1), constant pressure intake valve (2), gas unidirectional strainer valve (3), bubbling nozzle (16) and admission line;The reaction The side of kettle (7) is provided with air inlet, and top is provided with exhaust outlet;The gas outlet of the gas cylinder tank (1) passes through the air inlet Pipeline is sequentially connected the constant pressure intake valve (2), the air inlet and the bubbling nozzle (16), the bubbling nozzle (16) Positioned at the bottom of the reaction kettle (7);After the exhaust outlet connects the gas unidirectional strainer valve (3) by the admission line It accesses on the admission line between the air inlet and the constant pressure intake valve (2).
3. the quick equipment for continuously preparing gas hydrate according to claim 1 or 2, it is characterised in that:It is described to supply ice Liquid unit includes ice flow container (12), the ice liquid in the ice flow container (12) is broken into ultrasonic wave ice breaker and chipper (13), the ice of ice slurry Flow container valve (11), ice liquid pump (10), ice liquid inlet valve (8) and return line;The liquid outlet of the ice flow container (12) is by going out liquid Pipe is sequentially connected with ice flow container valve (11), ice liquid pump (10), ice liquid inlet valve (8) and accesses afterwards in the reaction kettle (7).
4. the quick equipment for continuously preparing gas hydrate according to claim 3, it is characterised in that:The hydrate mistake Filter all multi-layer filtrating equipments inside collector unit;The opposite side of the reaction kettle (7) passes through fast joint (14) and the hydration Unit connection is collected by filtration in object, and the rear end that unit is collected by filtration in the hydrate connects the quick-joint valve by the return line Door (15) accesses the ice flow container (12) afterwards.
5. the quick equipment for continuously preparing gas hydrate according to claim 1, it is characterised in that:The data acquisition Processing unit includes data acquisition processing device (4) and computer data processing system (5);The data acquisition processing device (4) including temperature sensor, pressure sensor and data acquisition control card;It is provided with and the temperature at the top of the reaction kettle (7) The temperature and pressure mouth that degree sensor, pressure sensor connect, the temperature sensor, pressure sensor are respectively connected to the data acquisition Control card, the data acquisition control card connect with the computer data processing system (5).
6. the quick equipment for continuously preparing gas hydrate according to claim 1, it is characterised in that:The reaction kettle (7) using autoclave (7).
7. the quick equipment for continuously preparing gas hydrate according to claim 4, it is characterised in that:The multiple filtration Device is using the vertically arranged filter screen of multilayer.
8. the quick equipment for continuously preparing gas hydrate according to claim 3, it is characterised in that:The temperature control Unit is constant temperature water bath (9).
CN201711297879.0A 2017-12-08 2017-12-08 A kind of quick equipment for continuously preparing gas hydrate Pending CN108160003A (en)

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CN201711297879.0A CN108160003A (en) 2017-12-08 2017-12-08 A kind of quick equipment for continuously preparing gas hydrate

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Application Number Priority Date Filing Date Title
CN201711297879.0A CN108160003A (en) 2017-12-08 2017-12-08 A kind of quick equipment for continuously preparing gas hydrate

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109731530A (en) * 2018-12-17 2019-05-10 中国科学院广州能源研究所 Electrostatic atomization acts on lower hydrate continuous generation device
CN109971519A (en) * 2019-03-28 2019-07-05 中国科学院广州能源研究所 The continuous preparation device of gas hydrates bead
CN110668628A (en) * 2019-10-15 2020-01-10 西南石油大学 Device and method for treating gas well production wastewater by hydrate method
CN111215019A (en) * 2018-11-27 2020-06-02 中国科学院广州能源研究所 Hydrate generation and sample preparation reation kettle part
CN112413959A (en) * 2020-11-24 2021-02-26 江门市新会区美亚化工有限公司 Production textile auxiliary uses high-efficient cooling device
CN112473571A (en) * 2020-10-28 2021-03-12 中石化宁波工程有限公司 Method capable of accelerating generation of gas hydrate in bubbling bed
CN114659312A (en) * 2022-03-30 2022-06-24 北京工业大学 Method for rapidly preparing carbon dioxide hydrate slurry for cold accumulation

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111215019A (en) * 2018-11-27 2020-06-02 中国科学院广州能源研究所 Hydrate generation and sample preparation reation kettle part
CN109731530A (en) * 2018-12-17 2019-05-10 中国科学院广州能源研究所 Electrostatic atomization acts on lower hydrate continuous generation device
WO2020124659A1 (en) * 2018-12-17 2020-06-25 中国科学院广州能源研究所 Apparatus for continuously generating hydrate under action of electrostatic atomization
CN109971519A (en) * 2019-03-28 2019-07-05 中国科学院广州能源研究所 The continuous preparation device of gas hydrates bead
WO2020192193A1 (en) * 2019-03-28 2020-10-01 中国科学院广州能源研究所 Apparatus for the continuous preparation of natural gas hydrate microsphere
CN110668628A (en) * 2019-10-15 2020-01-10 西南石油大学 Device and method for treating gas well production wastewater by hydrate method
CN112473571A (en) * 2020-10-28 2021-03-12 中石化宁波工程有限公司 Method capable of accelerating generation of gas hydrate in bubbling bed
CN112473571B (en) * 2020-10-28 2022-06-14 中石化宁波工程有限公司 Method capable of accelerating generation of gas hydrate in bubbling bed
CN112413959A (en) * 2020-11-24 2021-02-26 江门市新会区美亚化工有限公司 Production textile auxiliary uses high-efficient cooling device
CN114659312A (en) * 2022-03-30 2022-06-24 北京工业大学 Method for rapidly preparing carbon dioxide hydrate slurry for cold accumulation
CN114659312B (en) * 2022-03-30 2024-04-19 北京工业大学 Method for rapidly preparing carbon dioxide hydrate slurry for cold accumulation

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