CN102773042A - High temperature and high pressure reaction kettle provided with online sampling device - Google Patents
High temperature and high pressure reaction kettle provided with online sampling device Download PDFInfo
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- CN102773042A CN102773042A CN2012102908267A CN201210290826A CN102773042A CN 102773042 A CN102773042 A CN 102773042A CN 2012102908267 A CN2012102908267 A CN 2012102908267A CN 201210290826 A CN201210290826 A CN 201210290826A CN 102773042 A CN102773042 A CN 102773042A
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Abstract
The invention relates to a high temperature and high pressure reaction kettle provided with an online sampling device, and belongs to the technical field of chemical reacting equipment. The high temperature and high pressure reaction kettle provided with the online sampling device is structurally characterized in that a high temperature and high pressure kettle body (1) is communicated with a buffering kettle body (2) through a first sampling pipe (10), and a normal pressure and temperature kettle body (3) and the buffering kettle body (2) are communicated through a second sampling pipe (13). A heating, cooling and thermal insulation device, a vacuum device and a booster pump (7) which are arranged outside the high temperature and high pressure kettle body (1) supercharge pressurized gas. The first sampling pipe (10) is divided into two branches in the high temperature and high pressure kettle body (1) to sample gas samples and liquid samples respectively. The normal pressure and temperature kettle body (3) is provided with a gas outlet and a liquid outlet to be connected with detecting equipment. The high temperature and high pressure reaction kettle provided with the online sampling device is simple in structure, integrates online sampling, heating, supercharging and vacuuming into a whole, monitors reaction process through test by online sampling, accordingly problems during the reaction process can be dealt with as soon as possible, waste can be avoided, and good practical applicability is provided.
Description
Technical field
The invention belongs to the technical field that is used for chemical reaction device, be specifically related to a kind of high-temperature high-pressure reaction kettle with online sampler.
Background technology
Agitated reactor is a kind of equipment of realizing chemical reaction, is widely used in industries such as chemical industry, oil refining, metallurgy.The all direct-connected usually discharge nozzle of the discharging opening of existing equipment is directly delivered to next process with material, and the centre does not have monitoring device, can't monitor course of reaction and product.But in many courses of reaction such as chemical industry synthesizes; To material sample analysis in the agitated reactor is very important; Whether degree of not only can monitoring reaction carrying out and reaction are carried out according to the anticipation design, and can handle timely abnormal reaction, avoid waste.Do not carry out disclosing of real-time check and analysis mutually in the prior art to the gas-liquid in the HTHP stirred autoclave.
Summary of the invention
The technical problem that the present invention will solve is to deficiency of the prior art, a kind of high-temperature high-pressure reaction kettle with online sampler to be provided, to have the function of monitoring reaction process when realizing that this agitated reactor is reacted under high-temperature and high-pressure conditions.
In order to realize the foregoing invention purpose, the technical scheme that the present invention adopts is: a kind of high-temperature high-pressure reaction kettle with online sampler.This HTHP circulation blender gas liquid phase reactor still comprises the HTHP kettle, the buffering kettle, and the normal temperature and pressure kettle, agitator feeds the inner probe tube of high-temperature high-pressure reaction kettle, heating, cooling and attemperator, vacuum plant and the pressue device of kettle outside.Feed the inner probe tube of high-temperature high-pressure reaction kettle and be divided into two: a terminal is positioned at the agitated reactor inner and upper, gets gas appearance; Another terminal is positioned at below, agitated reactor inside, gets liquid-like.Pressue device is furnished with booster pump.All these devices are integrated in the automatic control box, through touch-screen control parameter and reaction process.
Concrete technical scheme is following:
A kind of high-temperature high-pressure reaction kettle with online sampler comprises the HTHP kettle 1 that has liquid inlet opening and gas feed(raw material)inlet, heating, cooling and attemperator outside the HTHP kettle 1, and pressue device; It is characterized in that structure cushions kettle 2 and normal temperature and pressure kettle 3 in addition; Between HTHP kettle 1 and buffering kettle 2, there is first probe tube 10 to be communicated with, between buffering kettle 2 and normal temperature and pressure kettle 3, has second probe tube 13 to be communicated with; Described first probe tube 10; Valve is equipped with in the centre; One end inserts in the buffering kettle 2; The other end also connects gas sample tube 5 and liquid sampling pipe 6, and gas appearance is got at the top of the opening of gas sample tube 5 in HTHP kettle 1, and liquid-like is got in the bottom of the opening of liquid sampling pipe 6 in HTHP kettle 1; Described second probe tube 13; Valve is equipped with in the centre, and an end inserts in the normal temperature and pressure kettle 3, and the other end also connects probe tube 11 and following probe tube 12; The opening of last probe tube 11 is got gas appearance at the top of buffering kettle 2, and the opening of following probe tube 12 is got liquid-like in the bottom of buffering kettle 2; Described normal temperature and pressure kettle 3, top have gas vent and are connected with checkout equipment, and the bottom has liquid outlet to be connected with checkout equipment; Described pressue device has the air pipe of adding, pressurized-gas source and booster pump 7, and an end that adds air pipe feeds in the HTHP kettle 1, and the other end is connected pressurized-gas source through gas valve with booster pump 7.
HTHP kettle 1 can be provided with electric mixer 4; Outside HTHP kettle 1, vavuum pump 8 can be set, vavuum pump 8 communicates in gas valve and HTHP kettle 1.These devices can be realized the stirring of HTHP kettle 1, the function that vacuumizes, and cooperate control device to realize control automatically.
Described buffering kettle 2 is equipped with vacuum extractor, and the temperature and pressure during work in the kettle is lower than HTHP kettle 1 and is higher than normal temperature and pressure kettle 3.
Above-mentioned high-temperature high-pressure reaction kettle with online sampler, described HTHP kettle 1 is equipped with air gauge, in heating, cooling and attemperator, temperature probe is housed; Described buffering kettle 2 is equipped with temperature sensor and pressure sensor.These detect sensing device and are used for each kettle technological parameter is detected and control automatically.Automatic control box 9 is arranged outside the HTHP kettle 1; Online sampling control equipment is housed in the automatic control box 9; The stirring control device of HTHP kettle 1, temperature control equipment, pressure control device, vacuumize control device, and the display unit of the temperature and pressure of buffering kettle 2.Can realization response process, online sampling, heat, pressurize, vacuumize, the automatic control of stirring etc.
Above-mentioned high-temperature high-pressure reaction kettle with online sampler; Being communicated with HTHP kettle 1 can be needle-valve with the valve that first probe tube 10 that cushions kettle 2 is provided with, and the valve that second probe tube 13 of connection buffering kettle 2 and normal temperature and pressure kettle 3 is provided with can be a needle-valve.The sampling material gets into buffering kettle 2 through probe tube and cushions, and then gets into normal temperature and pressure kettle 3 detection of taking a sample.On gas sample tube 5 and liquid sampling pipe 6, be respectively equipped with needle-valve; On last probe tube 11 and following probe tube 12, be respectively equipped with needle-valve.Above-mentioned all needle-valves are used to control sampling process and sampling amount.
High-temperature high-pressure reaction kettle with online sampler of the present invention is simple in structure; Integrate online sampling, stirring, heating, pressurize, vacuumize; Through the material that obtains from sample tap is chemically examined the monitoring reaction process, so that through real-time analysis, the problem that in time occurs in the processing reaction process; Avoid waste, have good economic outlook.
Description of drawings
Fig. 1 is the structural representation with high-temperature high-pressure reaction kettle of online sampler of the present invention.
The specific embodiment
Embodiment 1
Below in conjunction with accompanying drawing the present invention is done further explanation.
As shown in Figure 1, be the high-temperature high-pressure reaction kettle with online sampler of the present invention.Wherein, 1 is the HTHP kettle, and 2 are the buffering kettle, and 3 is the normal temperature and pressure kettle; 4 is electric mixer, and 5 is gas sample tube, and 6 is the liquid sampling pipe, and 7 is booster pump; Be used to gas-pressurized (the being generally nitrogen) supercharging that gets into HTHP kettle 1,8 is vavuum pump, and 9 is automatic control box, and 10 is first probe tube; 11 is last probe tube, and 12 are following probe tube, and 13 is second probe tube.
This high-temperature high-pressure reaction kettle with online sampler comprises the HTHP kettle 1 that can add liquid charging stock (through liquid inlet opening) and gas raw material (through the gas raw material inlet); Be used to alleviate the buffering kettle 2 that detects probe temperature pressure, be used to detect the normal temperature and pressure kettle 3 of sampling; HTHP kettle 1 has first probe tube 10 to communicate with 2 of kettlies of buffering, and buffering kettle 2 has second probe tube 13 to communicate with 3 of normal temperature and pressure kettlies.HTHP kettle 1 is provided with electric mixer 4, is connected with vacuum plant, vacuum plant is equipped with vavuum pump 8; At the bottom of still top and still, be provided with gas sample tube 5 and liquid sampling pipe 6, gas sample tube 5 is sent the sample that extracts into buffering kettle 2 after coming together in first probe tube 10 with liquid sampling pipe 6; HTHP kettle 1 outside is provided with heater, cooling device and attemperator, and pressue device; Pressue device comprises the booster pump 7 that adds air pipe, pressurized-gas source and configuration.Cushion kettle 2, the display unit of vacuum extractor, temperature and pressure can be housed.Normal temperature and pressure kettle 3 tops have gas vent, liquid outlet is arranged at the bottom, and they are connected with checkout equipment.The control of all these devices can be integrated in the automatic control box 9, through touch-screen control parameter and reaction process.
HTHP kettle 1 outer heating, cooling and attemperator adopts existing heat tracing structure and facility, and cooling device feeds cooling water for can use serpentine coil in the pipe.
Unstrpped gas and gas-pressurized can feed HTHP kettle 1 through same pipeline.Concrete structure can be: an end that adds air pipe feeds in the HTHP kettle 1, and the other end is divided into two-way, and one the tunnel is connected pressurized-gas source through gas valve with booster pump 7, and another road is through gas valve connection unstripped gas body source.Unstrpped gas and gas-pressurized can use the structure of same pipeline also can be stated as: described gas raw material inlet, communicate with adding air pipe, and unstrpped gas adds air pipe through the valve entering and gets in the HTHP kettle 1 again.
1), vavuum pump 8 vacuumizes reaction and testing process:; 2), add liquid charging stock through liquid inlet opening; Add gas raw material through the gas raw material inlet; 3), stir, temperature is set, heat up; 4), be raised to design temperature after, through booster pump 7 nitrogen pressure; 6), be added to setting pressure after, close booster pump 7, reaction beginning; 7), when getting gas and liquid-like, open the needle-valve of gas sample tube 5 and liquid sampling pipe 6 respectively, behind buffering kettle 2, get in the normal temperature and pressure kettle 3 the sampling detection; 8, after reaction finished, logical condensed water was reduced to room temperature, and still is driven in release.
The temperature range of the work of the HTHP kettle 1 among the present invention is: room temperature～400 ℃, working pressure range is: 10
3～3 * 10
7Pa.
An end that adds air pipe feeds HTHP kettle 1, and the other end can connect an interface of threeway, and two interfaces in addition of threeway connect pressurized-gas source and reacting gas source through needle-valve respectively.
In first probe tube, the 10 1 ends entering buffering kettle 2, the other end is split up into gas sample tube 5 and 6 two branches of liquid sampling pipe, also can adopt threeway to realize separating of gas sample tube 5 and liquid sampling pipe 6.
In second probe tube, the 13 1 ends entering buffering kettle 2, the other end is split up into gas sample tube 11 and 12 two branches of liquid sampling pipe, also can adopt threeway to realize separating of gas sample tube 11 and liquid sampling pipe 12.
Claims (5)
1. the high-temperature high-pressure reaction kettle with online sampler comprises the HTHP kettle (1) that has liquid inlet opening and gas feed(raw material)inlet, heating, cooling and attemperator that HTHP kettle (1) is outer, and pressue device; It is characterized in that structure cushions kettle (2) and normal temperature and pressure kettle (3) in addition; Between HTHP kettle (1) and buffering kettle (2), there is first probe tube (10) to be communicated with, between buffering kettle (2) and normal temperature and pressure kettle (3), has second probe tube (13) to be communicated with; Described first probe tube (10); Valve is equipped with in the centre; One end inserts in the buffering kettle (2); The other end also connects gas sample tube (5) and liquid sampling pipe (6), and gas appearance is got at the top of the opening of gas sample tube (5) in HTHP kettle (1), and liquid-like is got in the bottom of the opening of liquid sampling pipe (6) in HTHP kettle (1); Described second probe tube (13); Valve is equipped with in the centre; One end inserts in the normal temperature and pressure kettle (3); The other end also connects probe tube (11) and following probe tube (12), and the opening of last probe tube (11) is got gas appearance at the top of buffering kettle (2), and the opening of following probe tube (12) is got liquid-like in the bottom of buffering kettle (2); Described normal temperature and pressure kettle (3), top have gas vent and are connected with checkout equipment, and the bottom has liquid outlet to be connected with checkout equipment; Described pressue device has the air pipe of adding, pressurized-gas source and booster pump (7), and an end that adds air pipe feeds in the HTHP kettle (1), and the other end is connected pressurized-gas source through gas valve with booster pump (7).
2. the high-temperature high-pressure reaction kettle with online sampler according to claim 1 is characterized in that, HTHP kettle (1) is provided with electric mixer (4); Vavuum pump (8) is set outside HTHP kettle (1), and vavuum pump (8) communicates in gas valve and HTHP kettle (1).
3. the high-temperature high-pressure reaction kettle with online sampler according to claim 1 and 2 is characterized in that, on HTHP kettle (1), air gauge is housed, and in heating, cooling and attemperator, temperature probe is housed; At buffering kettle (2) temperature sensor and pressure sensor are housed; Automatic control box (9) is arranged outside the HTHP kettle (1); Automatic control box is equipped with online sampling control equipment in (9); The stirring control device of HTHP kettle (1), temperature control equipment, pressure control device, vacuumize control device, and the display unit of the temperature and pressure of buffering kettle (2).
4. the high-temperature high-pressure reaction kettle with online sampler according to claim 1 and 2 is characterized in that, on gas sample tube (5) and liquid sampling pipe (6), is respectively equipped with needle-valve; On last probe tube (11) and following probe tube (12), be respectively equipped with needle-valve.
5. the high-temperature high-pressure reaction kettle with online sampler according to claim 1 and 2 is characterized in that, described gas raw material inlet communicates with adding air pipe, and unstrpped gas adds air pipe through the valve entering and gets in the HTHP kettle (1) again.
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| CN201210290826.7A CN102773042B (en) | 2012-08-15 | 2012-08-15 | High temperature and high pressure reaction kettle provided with online sampling device |
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| CN201210290826.7A CN102773042B (en) | 2012-08-15 | 2012-08-15 | High temperature and high pressure reaction kettle provided with online sampling device |
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| CN102773042A true CN102773042A (en) | 2012-11-14 |
| CN102773042B CN102773042B (en) | 2015-04-08 |
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| CN103064437A (en) * | 2012-12-31 | 2013-04-24 | 广东电网公司电力科学研究院 | Device and method for controlling dissolved oxygen in reaction container |
| CN103521153A (en) * | 2013-07-25 | 2014-01-22 | 无锡意凯自动化技术有限公司 | Parallel reactor device |
| CN104459055A (en) * | 2014-12-19 | 2015-03-25 | 中国石油大学(华东) | Experimental device for high temperature and high pressure anti-corrosion reaction |
| CN105080427A (en) * | 2015-07-24 | 2015-11-25 | 河南理工大学 | High-temperature high-pressure water-cooled weighable reactor |
| CN105092409A (en) * | 2015-08-24 | 2015-11-25 | 江苏苏博特新材料股份有限公司 | Test device and detection method for testing cement and emulsified asphalt adsorption rates |
| CN106119084A (en) * | 2016-08-23 | 2016-11-16 | 上海交通大学 | Not pressure release continuous sampling formula high pressure microbial cultivation device |
| CN106153831A (en) * | 2016-08-17 | 2016-11-23 | 东北大学 | A kind of material meets tester and the method for wet generation fuel gas |
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| CN107727805A (en) * | 2017-10-18 | 2018-02-23 | 中石化炼化工程（集团）股份有限公司 | HTHP gas-liquid phase equilibrium test device and method |
| CN108267495A (en) * | 2017-11-28 | 2018-07-10 | 荆门市格林美新材料有限公司 | The system and method for oxygen content during a kind of monitoring multicomponent material precursor synthesis |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN202284988U (en) * | 2011-10-10 | 2012-06-27 | 恒升化工（启东）有限公司 | Pressurized liquid sampling device |
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2012
- 2012-08-15 CN CN201210290826.7A patent/CN102773042B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN202284988U (en) * | 2011-10-10 | 2012-06-27 | 恒升化工（启东）有限公司 | Pressurized liquid sampling device |
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| CN103064437B (en) * | 2012-12-31 | 2015-06-24 | 广东电网公司电力科学研究院 | Device and method for controlling dissolved oxygen in reaction container |
| CN103064437A (en) * | 2012-12-31 | 2013-04-24 | 广东电网公司电力科学研究院 | Device and method for controlling dissolved oxygen in reaction container |
| CN103521153A (en) * | 2013-07-25 | 2014-01-22 | 无锡意凯自动化技术有限公司 | Parallel reactor device |
| CN103521153B (en) * | 2013-07-25 | 2015-11-18 | 无锡意凯自动化技术有限公司 | A kind of parallel reaction apparatus |
| CN104459055A (en) * | 2014-12-19 | 2015-03-25 | 中国石油大学(华东) | Experimental device for high temperature and high pressure anti-corrosion reaction |
| CN104459055B (en) * | 2014-12-19 | 2016-03-30 | 中国石油大学(华东) | A kind of high-temperature high-pressure corrosion resisting reaction experiment device and on reactor System Utilization Procedure |
| CN106179122A (en) * | 2015-04-30 | 2016-12-07 | 中国石油化工股份有限公司 | The consersion unit of alkadienes and application thereof |
| CN106179122B (en) * | 2015-04-30 | 2019-06-28 | 中国石油化工股份有限公司 | The consersion unit of alkadienes and its application |
| CN105080427A (en) * | 2015-07-24 | 2015-11-25 | 河南理工大学 | High-temperature high-pressure water-cooled weighable reactor |
| CN105092409B (en) * | 2015-08-24 | 2017-10-10 | 江苏苏博特新材料股份有限公司 | It is a kind of to test cement and the test device and detection method of emulsified asphalt adsorption rate |
| CN105092409A (en) * | 2015-08-24 | 2015-11-25 | 江苏苏博特新材料股份有限公司 | Test device and detection method for testing cement and emulsified asphalt adsorption rates |
| CN106153831A (en) * | 2016-08-17 | 2016-11-23 | 东北大学 | A kind of material meets tester and the method for wet generation fuel gas |
| CN106119084A (en) * | 2016-08-23 | 2016-11-16 | 上海交通大学 | Not pressure release continuous sampling formula high pressure microbial cultivation device |
| CN107727805A (en) * | 2017-10-18 | 2018-02-23 | 中石化炼化工程（集团）股份有限公司 | HTHP gas-liquid phase equilibrium test device and method |
| CN107727805B (en) * | 2017-10-18 | 2021-06-08 | 中石化炼化工程（集团）股份有限公司 | High-temperature high-pressure gas-liquid phase balance testing device and method |
| CN108267495A (en) * | 2017-11-28 | 2018-07-10 | 荆门市格林美新材料有限公司 | The system and method for oxygen content during a kind of monitoring multicomponent material precursor synthesis |
| CN112266861A (en) * | 2020-09-14 | 2021-01-26 | 中国石油天然气股份有限公司 | Oil reservoir microorganism storage and transportation device and application |
| CN112985925A (en) * | 2021-02-24 | 2021-06-18 | 吉林大学 | Automatic sampling and collecting device |
| CN113856586A (en) * | 2021-08-20 | 2021-12-31 | 中国原子能科学研究院 | Device for gas-liquid conversion and gas-liquid two-phase online sampling of iodine |
| CN113856586B (en) * | 2021-08-20 | 2022-12-13 | 中国原子能科学研究院 | Device for gas-liquid conversion and gas-liquid two-phase online sampling of iodine |
| CN114733446A (en) * | 2022-05-17 | 2022-07-12 | 吉林大学 | But high temperature high pressure batch autoclave of normal position monitoring resistance |
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