CN111215019A - Hydrate generation and sample preparation reation kettle part - Google Patents
Hydrate generation and sample preparation reation kettle part Download PDFInfo
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- CN111215019A CN111215019A CN201811422427.5A CN201811422427A CN111215019A CN 111215019 A CN111215019 A CN 111215019A CN 201811422427 A CN201811422427 A CN 201811422427A CN 111215019 A CN111215019 A CN 111215019A
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- reaction kettle
- kettle
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- hydrate
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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
- B01J19/28—Moving reactors, e.g. rotary drums
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F29/00—Mixers with rotating receptacles
- B01F29/60—Mixers with rotating receptacles rotating about a horizontal or inclined axis, e.g. drum mixers
- B01F29/62—Mixers with rotating receptacles rotating about a horizontal or inclined axis, e.g. drum mixers without bars, i.e. without mixing elements; characterised by the shape or cross section of the receptacle, e.g. of Y-, Z-, S- or X- shape; with cylindrical receptacles rotating about an axis at an angle to their longitudinal axis
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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
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/04—Pressure vessels, e.g. autoclaves
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a hydrate generation and sample preparation reaction kettle component, which comprises a reaction kettle, a kettle cover, a pressure and temperature monitoring device and a frequency-adjustable rotating motor, wherein the reaction kettle is provided with a cavity; one side of the reaction kettle is provided with an air inlet pipeline and an air inlet valve, and the other side of the reaction kettle is provided with a liquid inlet pipeline and a liquid inlet valve; the pipe wall of the gas inlet pipeline positioned in the reaction kettle is densely distributed with small holes; the inner side surface and the outer side surface of the reaction kettle are plated with nano titanium composite plating layers; the pressure and temperature monitoring device comprises a pressure monitor meter and a temperature monitor meter; the frequency-adjustable rotating motor comprises a positive and negative rotating motor capable of rotating positively and negatively and a motor frequency modulator connected with the positive and negative rotating motor; the reaction kettle is arranged on the stainless steel bracket, and the whole reaction kettle part is arranged in a constant temperature air bath with programmable temperature control; the reaction kettle is provided with a vacuum instrument. The device can effectively improve the reaction rate of the hydrate and simultaneously ensure the uniformity and compactness of a generated hydrate sample; the reaction rate is high, the surface of the sample is smooth, and the sample is uniformly distributed.
Description
Technical Field
The invention relates to the technical field of hydrate production and preparation, in particular to a hydrate generation and sample preparation reaction kettle component.
Background
The gas hydrate is a cage-type crystalline compound with different guest molecules such as CH4，CO2，N2，H2When the gas and water are at low temperature and high temperatureDifferent types of gas hydrates can be formed under pressure conditions. The hydrate can be applied to different industrial technical fields by utilizing the difference of the cage structure of the hydrate and the conditions for forming the hydrate by various guest molecules. However, basic research of hydrates requires test analysis and characterization of hydrate samples, and characterization of hydrate samples requires comprehensive multi-scale test analysis of different samples by using related equipment, and these multi-scale test analyses have relatively high requirements on hydrate samples and require that the generated hydrate samples have compact uniformity, so that the reaction process of the hydrate samples requires complete reaction of water and gas.
At present, common hydrate sample reaction devices are all focused on stirring modes in a kettle, such as mechanical stirring, magnetic stirring, top spraying and the like, the modes can effectively increase the contact surface between liquid and gas, and can promote the generation of hydrates to a certain extent, but certain disadvantages exist. For example, in the case of the stirring mode, when the hydrate formation rate is high, the stirring can be blocked and stopped, and the existence of the rotating blade and the stirring bar can influence the compactness and uniformity of the hydrate sample; in the case of the top shower, the generation of hydrate is promoted by the initial liquid shower, but the amount of the liquid to be sprayed is fixed, and the promotion effect of the top shower is substantially lost after the liquid required for the reaction is completely sprayed.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a hydrate generation and sample preparation reaction kettle component.
The invention is realized by the following technical scheme: a hydrate generation and sample preparation reaction kettle component comprises a reaction kettle, a kettle cover, a pressure and temperature monitoring device and a frequency-adjustable rotating motor; one side of the reaction kettle is provided with an air inlet pipeline and an air inlet valve, and the other side of the reaction kettle is provided with a liquid inlet pipeline and a liquid inlet valve; the pipe wall of the gas inlet pipeline positioned in the reaction kettle is densely distributed with small holes; the inner side surface and the outer side surface of the reaction kettle are plated with nano titanium composite plating layers; the kettle cover is connected with the reaction kettle through a buckle, and the kettle cover is connected with the reaction kettle through threads and sealed through a rubber ring; the pressure and temperature monitoring device comprises a pressure monitor meter and a temperature monitor meter; the frequency-adjustable rotating motor comprises a positive and negative rotating motor capable of rotating positively and negatively and a motor frequency modulator connected with the positive and negative rotating motor; the side wall of the reaction kettle is provided with a strip-shaped window; the reaction kettle is placed on a stainless steel bracket, and the whole reaction kettle part is placed in a constant-temperature air bath with programmable temperature control; the reaction kettle is provided with a vacuum instrument.
The pipe wall of the gas inlet pipeline is densely distributed with small holes, so that gas begins to diffuse immediately after entering the reaction kettle, and the contact area of the gas and the liquid is increased; the positive and negative rotation motor can rotate the reaction kettle in a positive-negative two-way manner, can effectively drive the liquid in the reaction kettle to turn over, increases the contact area of the liquid and the gas, and improves the conversion rate of the hydrate; the arrangement of the strip-shaped window can observe the internal condition of the reaction kettle at any time; the surface of the reaction kettle is plated with the nano titanium composite plating layer to improve the heat conductivity and promote the heat transfer required by the generation of the hydrate. Meanwhile, the coating has corrosion resistance and is suitable for various kinds of work and working conditions; the pressure monitor meter and the temperature monitor meter are used for monitoring the temperature and the pressure condition in the reaction kettle in real time; the whole reaction kettle component is placed in a constant-temperature air bath and can be used for carrying out hydrate generation and sample preparation reaction; the vacuum instrument is used for observing the vacuum state in the reaction kettle.
The inner wall of the reaction kettle is provided with strip fins, and small holes are densely distributed in the strip fins. The fins are densely distributed with small holes for dividing fluid, slowing down the movement speed of the fluid and increasing the contact surface of the fluid and gas.
The diameter of the small holes of the strip-shaped fins is 5 mm.
The strip-shaped window is made of high-pressure-resistant organic glass materials. The strip-shaped window made of the high-pressure-resistant organic glass material can effectively withstand pressure and ensure the sealing of the reaction kettle, and can observe the internal condition of the reaction kettle in real time.
The reaction kettle is made of a high-pressure-resistant and corrosion-resistant stainless steel material.
The bottom of reation kettle with the kettle cover all is equipped with outstanding branch, the confession has been seted up to the stainless steel support branch male circular socket. The stainless steel support can effectively support the reaction kettle and ensure that the reaction kettle can smoothly rotate forwards and backwards while not shaking.
Compared with the prior art, the invention has the advantages that: the device overcomes the defects of the existing hydrate reaction kettle, provides a novel hydrate sample reaction kettle component, can effectively improve the reaction rate of the hydrate, and simultaneously ensures the uniformity and compactness of the generated hydrate sample; the problems of slow reaction rate in the process of generating the hydrate sample, unsmooth sample surface and nonuniform sample distribution are solved.
Drawings
Fig. 1 is a schematic structural diagram of an embodiment of the present invention.
The reference numerals in the drawings mean: 1. a reaction kettle; 2. a temperature monitoring instrument; 3. a positive and negative rotation rotating motor; 4. a motor frequency modulator; 5. a strip-shaped window; 6. strip-shaped fins; 7. a flange hoop; 8. a kettle cover; 9. a vacuum gauge; 10. a pressure monitoring instrument; 11. a reaction solution; 12. a stainless steel bracket; v1, a liquid inlet valve; v2, air inlet valve.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and detailed description.
Examples
Referring to fig. 1, a hydrate generating and sample preparing reaction kettle 1 component comprises a reaction kettle 1, a kettle cover 8, a pressure and temperature monitoring device, and a frequency-adjustable rotating motor; one side of the reaction kettle 1 is provided with an air inlet pipeline and an air inlet valve V2, and the other side is provided with a liquid inlet pipeline and a liquid inlet valve V1; the pipe wall of the gas inlet pipeline positioned in the reaction kettle 1 is densely distributed with small holes; the inner side surface and the outer side surface of the reaction kettle 1 are plated with nano titanium composite plating layers; the kettle cover 8 is connected with the reaction kettle 1 through a buckle, and the kettle cover 8 is connected with the reaction kettle 1 through threads and sealed through a rubber ring; the pressure and temperature monitoring device comprises a pressure monitoring instrument 10 and a temperature monitoring instrument 2; the frequency-adjustable rotating motor comprises a positive and negative rotating motor 3 capable of rotating positively and negatively and a motor frequency modulator 4 connected with the positive and negative rotating motor; the side wall of the reaction kettle 1 is provided with a strip-shaped window 5; the reaction kettle 1 is arranged on a stainless steel bracket 12, and the whole reaction kettle 1 part is arranged in a constant temperature air bath with programmable temperature control; the reaction kettle 1 is provided with a vacuum instrument 9.
The pipe wall of the gas inlet pipeline is densely distributed with small holes, so that gas begins to diffuse immediately after entering the reaction kettle 1, and the contact area of the gas and the liquid is increased; the positive and negative rotation rotating motor 3 can rotate the reaction kettle 1 in a positive-negative two-way manner, can effectively drive the liquid in the reaction kettle 1 to overturn, increases the contact area of the liquid and the gas, and improves the conversion rate of the hydrate; the arrangement of the strip-shaped window 5 can observe the internal condition of the reaction kettle 1 at any time; the surface of the reaction kettle 1 is plated with the nano titanium composite plating layer to improve the heat conductivity and promote the heat transfer required by the generation of the hydrate. Meanwhile, the coating has corrosion resistance and is suitable for various kinds of work and working conditions; the pressure monitoring instrument 10 and the temperature monitoring instrument 2 are used for monitoring the temperature and the pressure condition in the reaction kettle 1 in real time; the whole reaction kettle 1 part is placed in a constant-temperature air bath and can be used for hydrate generation and sample preparation reaction; the vacuum gauge 9 is used for observing the vacuum state in the reaction kettle 1.
The inner wall of the reaction kettle 1 is provided with strip fins 6, and the strip fins 6 are densely distributed with small holes. The fins are densely distributed with small holes for dividing fluid, slowing down the movement speed of the fluid and increasing the contact surface of the fluid and gas.
The diameter of the small holes of the strip-shaped fins 6 is 5 mm.
The strip-shaped window 5 is made of high-pressure-resistant organic glass material. The strip-shaped window 5 made of high-pressure-resistant organic glass material can effectively withstand pressure and ensure that the reaction kettle 1 is sealed, and can observe the internal conditions of the reaction kettle 1 in real time.
The reaction kettle 1 is made of high-pressure-resistant and corrosion-resistant stainless steel materials and is a reaction kettle 1.
The bottom of the reaction kettle 1 and the kettle cover 8 are both provided with protruding support rods, and the stainless steel support 12 is provided with circular insertion openings for the support rods to be inserted. Stainless steel support 12 can guarantee that reation kettle 1 can be smooth positive and negative rotation when effectively supporting reation kettle 1 and not rocking.
In this embodiment, the reaction vessel 1 is connected to an external common related device to form a complete hydrate formation experimental apparatus.
When the vacuum reactor is used, firstly, the inside of the reaction kettle 1 is cleaned, then the reaction kettle 1 is placed on the stainless steel bracket 12, the air inlet valve V2 is opened, the reaction kettle 1 is vacuumized by an external vacuumizing device, and after about 5 minutes, when the vacuum instrument 9 shows that the inside of the kettle is in a basic vacuum state, the air inlet valve V2 is closed. The liquid inlet valve V1 is opened, the reaction solution 11 is sucked into the reaction kettle 1 by utilizing the negative pressure in the reaction kettle 1, and then the liquid inlet valve V1 is closed. The external air bath was turned on and the reaction temperature was set. Observing the temperature monitoring instrument 2, opening the air inlet valve V2 after the temperature in the reaction kettle 1 is constant, making high-pressure gas enter the reaction kettle 1 through an external gas source, determining the pressure in the kettle through the pressure monitoring instrument 10, and closing the air inlet valve V2 when the pressure reaches a preset value. And (4) turning on a rotating motor frequency modulator 4, setting the frequency of the rotating motor 3 rotating positively and negatively, and starting the hydrate reaction. The condition in the reaction kettle 1 is observed through the strip-shaped window 5 of the reaction kettle 1, the temperature monitoring instrument 2 and the pressure monitoring instrument 10, and the hydrate reaction is finished when the pressure is not changed any more. The reaction vessel 1 was taken out and placed in liquid nitrogen for 5 minutes, the flange yoke 7 and the vessel lid 8 (in this example, the vessel lid was fixed to one end of the reaction vessel 1 by the flange yoke 7) were opened, and a hydrate sample was taken out and stored in liquid nitrogen.
The application of this example is as follows:
the application (1): get CH4，CO2And N2The mixed gas of the three is used as hydrate generating gas, 1/3 distilled water in the volume of the reaction kettle 1 is used as liquid, the pressure is 10MPa, the temperature is 273K, the frequency of rotating the forward and reverse rotating motor 3 is 60 times/minute of forward and reverse rotation, and the pressure in the reaction kettle 1 is reduced to 4MPa after 2 hours of reaction. At this time, the reaction kettle 1 is opened, the distilled water in the reaction kettle 1 is completely converted into hydrate, and the sample is placed in liquid nitrogen for storage and then subjected to X-ray diffraction analysis (XRD), so that no crystal peak with ice appears.
The application (2): taking pure CH4Using 1/3 in the volume of reaction kettle 1 and Sodium Dodecyl Sulfate (SDS) water solution with concentration of 200ppm as liquid to perform hydrate formation reaction, wherein the pressure is 15MPa, the temperature is 273K, the frequency of rotating the rotating motor 3 is 60 times/minute, after 2h reaction, the reaction kettle 1 is filled with hydrateThe pressure drop was 8 MPa. At this time, the reaction vessel 1 was opened, the distilled water in the reaction vessel 1 was completely converted into a hydrate, and the sample was stored in liquid nitrogen for 1 day and then subjected to X-ray diffraction analysis (XRD), and no crystal peak with ice was found.
The above detailed description is specific to possible embodiments of the present invention, and the embodiments are not intended to limit the scope of the present invention, and all equivalent implementations or modifications that do not depart from the scope of the present invention are intended to be included within the scope of the present invention.
Claims (6)
1. A hydrate formation and sample preparation reation kettle part which characterized in that: comprises a reaction kettle, a kettle cover, a pressure and temperature monitoring device and a frequency-adjustable rotating motor; one side of the reaction kettle is provided with an air inlet pipeline and an air inlet valve, and the other side of the reaction kettle is provided with a liquid inlet pipeline and a liquid inlet valve; the pipe wall of the gas inlet pipeline positioned in the reaction kettle is densely distributed with small holes; the inner side surface and the outer side surface of the reaction kettle are plated with nano titanium composite plating layers; the kettle cover is connected with the reaction kettle through a buckle, and the kettle cover is connected with the reaction kettle through threads and sealed through a rubber ring; the pressure and temperature monitoring device comprises a pressure monitor meter and a temperature monitor meter; the frequency-adjustable rotating motor comprises a positive and negative rotating motor capable of rotating positively and negatively and a motor frequency modulator connected with the positive and negative rotating motor; the side wall of the reaction kettle is provided with a strip-shaped window; the reaction kettle is placed on a stainless steel bracket, and the whole reaction kettle part is placed in a constant-temperature air bath with programmable temperature control; the reaction kettle is provided with a vacuum instrument.
2. The hydrate formation and sample preparation reaction vessel component of claim 1, wherein: the inner wall of the reaction kettle is provided with strip fins, and small holes are densely distributed in the strip fins.
3. The hydrate formation and sample preparation reaction vessel component of claim 2, wherein: the diameter of the small holes of the strip-shaped fins is 5 mm.
4. The hydrate formation and sample preparation reaction vessel component of claim 1, wherein: the strip-shaped window is made of high-pressure-resistant organic glass materials.
5. The hydrate formation and sample preparation reaction vessel component of claim 1, wherein: the reaction kettle is made of a high-pressure-resistant and corrosion-resistant stainless steel material.
6. The hydrate formation and sample preparation reaction vessel component of claim 1, wherein: the bottom of reation kettle with the kettle cover all is equipped with outstanding branch, the confession has been seted up to the stainless steel support branch male circular socket.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811422427.5A CN111215019A (en) | 2018-11-27 | 2018-11-27 | Hydrate generation and sample preparation reation kettle part |
| PCT/CN2018/124175 WO2020107608A1 (en) | 2018-11-27 | 2018-12-27 | Reaction kettle component for hydrate generation and sample preparation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811422427.5A CN111215019A (en) | 2018-11-27 | 2018-11-27 | Hydrate generation and sample preparation reation kettle part |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111215019A true CN111215019A (en) | 2020-06-02 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811422427.5A Pending CN111215019A (en) | 2018-11-27 | 2018-11-27 | Hydrate generation and sample preparation reation kettle part |
Country Status (2)
| Country | Link |
|---|---|
| CN (1) | CN111215019A (en) |
| WO (1) | WO2020107608A1 (en) |
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| JP2006160833A (en) * | 2004-12-03 | 2006-06-22 | Mitsui Eng & Shipbuild Co Ltd | Apparatus and method for producing gas hydrate |
| CN102513052A (en) * | 2011-12-27 | 2012-06-27 | 西南石油大学 | Natural gas hydrate generating device capable of being quickly disassembled for sampling |
| KR101404068B1 (en) * | 2013-07-09 | 2014-06-09 | 동국대학교 산학협력단 | Gas hydrate cooling apparatus |
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| CN108160003A (en) * | 2017-12-08 | 2018-06-15 | 中国科学院广州能源研究所 | A kind of quick equipment for continuously preparing gas hydrate |
| CN207756155U (en) * | 2017-12-27 | 2018-08-24 | 珠海市泽涛粘合制品有限公司 | A kind of reaction kettle |
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| JPH0298407A (en) * | 1988-10-05 | 1990-04-10 | Marumi Touriyou Kk | Mixing device for raw material for title |
| CN101612539A (en) * | 2009-07-16 | 2009-12-30 | 上海理工大学 | A kind of low temperature high pressure gas hydrate replacement reaction kettle and system |
| CN201603545U (en) * | 2009-12-01 | 2010-10-13 | 广东省广州石油机械厂 | Hydrate experiment device |
| CN106669553A (en) * | 2016-12-26 | 2017-05-17 | 中国科学院广州能源研究所 | Reciprocating turning type experimental device for generating even gas hydrate |
| CN108169448B (en) * | 2017-12-06 | 2020-06-12 | 中国科学院广州能源研究所 | Hydrate in-situ synthesis and comprehensive physical property testing device thereof |
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2018
- 2018-11-27 CN CN201811422427.5A patent/CN111215019A/en active Pending
- 2018-12-27 WO PCT/CN2018/124175 patent/WO2020107608A1/en active Application Filing
Patent Citations (9)
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|---|---|---|---|---|
| JP2006160833A (en) * | 2004-12-03 | 2006-06-22 | Mitsui Eng & Shipbuild Co Ltd | Apparatus and method for producing gas hydrate |
| CN102513052A (en) * | 2011-12-27 | 2012-06-27 | 西南石油大学 | Natural gas hydrate generating device capable of being quickly disassembled for sampling |
| KR101404068B1 (en) * | 2013-07-09 | 2014-06-09 | 동국대학교 산학협력단 | Gas hydrate cooling apparatus |
| CN204275883U (en) * | 2014-11-24 | 2015-04-22 | 赣州市利华兽药有限公司 | A kind of veterinary drug dilution explosive barrel |
| CN105107429A (en) * | 2015-09-16 | 2015-12-02 | 大连理工大学 | Semi-continuous piston type hydrate cake generating device |
| CN106268520A (en) * | 2016-09-12 | 2017-01-04 | 西南石油大学 | Gas hydrates synthesis Wobble plate type reactor system |
| CN207081712U (en) * | 2017-08-25 | 2018-03-09 | 中国石油大学(华东) | It is a kind of to be used for experimental provision of the hydrate generation with suppressing research under flox condition |
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| CN207756155U (en) * | 2017-12-27 | 2018-08-24 | 珠海市泽涛粘合制品有限公司 | A kind of reaction kettle |
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| WO2020107608A1 (en) | 2020-06-04 |
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Application publication date: 20200602 |