CN102773042B - 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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- CN102773042B CN102773042B CN201210290826.7A CN201210290826A CN102773042B CN 102773042 B CN102773042 B CN 102773042B CN 201210290826 A CN201210290826 A CN 201210290826A CN 102773042 B CN102773042 B CN 102773042B
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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 for chemical reaction device, be specifically related to a kind of high-temperature high-pressure reaction kettle with on-line period device.
Background technology
Reactor is a kind of equipment realizing chemical reaction, is widely used in the industries such as chemical industry, oil refining, metallurgy.The discharging opening all direct-connected discharge nozzle usually of existing equipment, directly material is delivered to next process, centre does not have monitoring device, cannot monitor course of reaction and product.But in many courses of reaction such as chemical industry synthesis, very important to material sample analysis in reactor, not only can monitor and react the degree of carrying out and whether reaction is carried out according to anticipation design, and can process timely abnormal reaction, avoid waste.Do not carry out detecting disclosing of analysis in real time for the liquid phase in High Temperature High Pressure stirred autoclave in prior art.
Summary of the invention
The technical problem to be solved in the present invention is, for deficiency of the prior art, provides a kind of high-temperature high-pressure reaction kettle with on-line period device, while realizing making this reactor carry out reacting under high-temperature and high-pressure conditions, have the function of monitoring reaction process.
In order to realize foregoing invention object, the technical solution used in the present invention is: a kind of high-temperature high-pressure reaction kettle with on-line period device.This High Temperature High Pressure circulation stirring liquid phase reactor comprises High Temperature High Pressure kettle, and buffering kettle, normal temperature and pressure kettle, stirrer, passes into the stopple coupon of high-temperature high-pressure reaction kettle inside, the heating outside kettle, cooling and attemperator, vacuum plant and pressue device.The stopple coupon passing into high-temperature high-pressure reaction kettle inside is divided into two: terminal to be positioned at reactor inner upper, gets gas sample; Another terminal is positioned at reactor lower inside, gets liquid-like.Pressue device is furnished with supercharge pump.All these devices are integrated in automatic control box, by touch-screen controling parameters and reaction process.
Concrete technical scheme is as follows:
There is a high-temperature high-pressure reaction kettle for on-line period device, comprise the High Temperature High Pressure kettle 1 having liquid inlet opening and gas feed(raw material)inlet, the heating outside High Temperature High Pressure kettle 1, cooling and attemperator, and pressue device; It is characterized in that, structure also has buffering kettle 2 and normal temperature and pressure kettle 3; Between High Temperature High Pressure kettle 1 and buffering kettle 2, there is the first stopple coupon 10 to be communicated with, between buffering kettle 2 and normal temperature and pressure kettle 3, have the second stopple coupon 13 to be communicated with; The first described stopple coupon 10, valve is equipped with in centre, one end is inserted in buffering kettle 2, the other end also connects gas sample tube 5 and liquid sampling pipe 6, gas sample is got at the top of opening in High Temperature High Pressure kettle 1 of gas sample tube 5, and liquid-like is got in the bottom of opening in High Temperature High Pressure kettle 1 of liquid sampling pipe 6; The second described stopple coupon 13, valve is equipped with in centre, and one end is inserted in normal temperature and pressure kettle 3, and the other end also connects stopple coupon 11 and lower stopple coupon 12, the opening of upper stopple coupon 11 gets gas sample at the top of buffering kettle 2, and the opening of lower stopple coupon 12 gets liquid-like in the bottom of buffering kettle 2; Described normal temperature and pressure kettle 3, top has gas vent and is connected with checkout equipment, and bottom has liquid outlet to be connected with checkout equipment; Described pressue device, has and adds air pipe, pressurized-gas source and supercharge pump 7, and the one end adding air pipe passes in High Temperature High Pressure kettle 1, and the other end is connected pressurized-gas source through gas valve with supercharge pump 7.
High Temperature High Pressure kettle 1 can arrange electric mixer 4; Can arrange vacuum pump 8 outside High Temperature High Pressure kettle 1, vacuum pump 8 communicates with in High Temperature High Pressure kettle 1 through gas valve.The stirring that these devices can realize High Temperature High Pressure kettle 1, the function vacuumized, and coordinate control device to realize automatically controlling.
Described buffering kettle 2, is equipped with vacuum extractor, temperature and pressure during work in kettle lower than High Temperature High Pressure kettle 1 higher than normal temperature and pressure kettle 3.
The above-mentioned high-temperature high-pressure reaction kettle with on-line period device, described High Temperature High Pressure kettle 1 is equipped with rain glass, in heating, cooling and attemperator, temperature probe is housed; Described buffering kettle 2 is equipped with temperature sensor and pressure transducer.These detect sensing device and are used for carrying out detection to each kettle technological parameter and automatically controlling.Automatic control box 9 is had outside High Temperature High Pressure kettle 1, automatic control box 9 is built with on-line period control device, mixing control device, temperature control equipment, the pressure control device of High Temperature High Pressure kettle 1, vacuumize control device, and the display device of the temperature and pressure of buffering kettle 2.Can realization response process, on-line period, heat, pressurize, vacuumize, the automatic control of stirring etc.
The above-mentioned high-temperature high-pressure reaction kettle with on-line period device, the valve that the first stopple coupon 10 being communicated with High Temperature High Pressure kettle 1 and buffering kettle 2 is provided with can be needle-valve, and the valve that the second stopple coupon 13 being communicated with buffering kettle 2 and normal temperature and pressure kettle 3 is provided with can be needle-valve.Sampling material by stopple coupon enter buffering kettle 2 cushion, and then enter normal temperature and pressure kettle 3 carry out sampling detection.Gas sample tube 5 and liquid sampling pipe 6 are respectively equipped with needle-valve; Upper stopple coupon 11 and lower stopple coupon 12 are respectively equipped with needle-valve.Above-mentioned all needle-valves are for controlling sampling process and sampling amount.
The high-temperature high-pressure reaction kettle structure with on-line period device of the present invention is simple, integrate on-line period, stirring, heating, pressurize, vacuumize, reaction process is monitored by carrying out chemical examination to the material obtained from sample tap, to pass through real-time analysis, produced problem in timely processing reaction process, avoid waste, there is good economic outlook.
Accompanying drawing explanation
Fig. 1 is the structural representation with the high-temperature high-pressure reaction kettle of on-line period device of the present invention.
Embodiment
Embodiment 1
Below in conjunction with accompanying drawing, the present invention will be further explained.
As shown in Figure 1, be the high-temperature high-pressure reaction kettle with on-line period device of the present invention.Wherein, 1 is High Temperature High Pressure kettle, and 2 is buffering kettle, 3 is normal temperature and pressure kettle, and 4 is electric mixer, and 5 is gas sample tube, 6 is liquid sampling pipe, and 7 is supercharge pump, for gas-pressurized (the being generally nitrogen) supercharging for entering High Temperature High Pressure kettle 1,8 is vacuum pump, 9 is automatic control box, and 10 is the first stopple coupon, and 11 is upper stopple coupon, 12 is lower stopple coupon, and 13 is the second stopple coupon.
This high-temperature high-pressure reaction kettle with on-line period device comprises the High Temperature High Pressure kettle 1 that can add liquid charging stock (through liquid inlet opening) and gas raw material (through gas raw material entrance), for alleviating the buffering kettle 2 detecting probe temperature pressure, for detecting the normal temperature and pressure kettle 3 of sampling; Have the first stopple coupon 10 to communicate between High Temperature High Pressure kettle 1 with buffering kettle 2, buffering kettle 2 communicates with there being the second stopple coupon 13 between normal temperature and pressure kettle 3.High Temperature High Pressure kettle 1 is provided with electric mixer 4, is connected with vacuum plant, vacuum plant is equipped with vacuum pump 8, at the bottom of still top and still, be provided with gas sample tube 5 and liquid sampling pipe 6, after gas sample tube 5 and liquid sampling pipe 6 come together in the first stopple coupon 10, the sample extracted sent into buffering kettle 2; Heating arrangement, cooling device and attemperator is provided with outside High Temperature High Pressure kettle 1, and pressue device; Pressue device comprises the supercharge pump 7 adding air pipe, pressurized-gas source and configuration.Buffering kettle 2, can be equipped with the display device of vacuum extractor, temperature and pressure.Normal temperature and pressure kettle 3 top has gas vent, liquid outlet is arranged at bottom, and they are connected with checkout equipment.The control of all these devices can be integrated in automatic control box 9, by touch-screen controling parameters and reaction process.
Heating outside High Temperature High Pressure kettle 1, cooling and attemperator adopt existing heating and thermal insulation structure and facility, and cooling device, for can use sinuous coil, passes into chilled water in pipe.
Unstrpped gas and gas-pressurized can pass into High Temperature High Pressure kettle 1 by same pipeline.Concrete structure can be: the one end adding air pipe passes in High Temperature High Pressure kettle 1, and the other end is divided into two-way, and a road is connected pressurized-gas source through gas valve with supercharge pump 7, and another road connects unstripped gas body source through gas valve.Unstrpped gas and gas-pressurized can use the structure of same pipeline also can be stated as: described gas raw material entrance, and add air pipe and communicate, and unstrpped gas enters through valve and adds air pipe and enter in High Temperature High Pressure kettle 1 again.
Reaction and testing process: 1), vacuum pump 8 vacuumizes; 2), liquid charging stock is added by liquid inlet opening; Gas raw material is added by gas raw material entrance; 3), stir, set temperature, heat up; 4), be raised to design temperature after, by supercharge pump 7 nitrogen pressurization; 6), be added to set pressure after, close supercharge pump 7, reaction start; 7), when getting gas and liquid-like, open the needle-valve of gas sample tube 5 and liquid sampling pipe 6 respectively, after buffering kettle 2, enter in normal temperature and pressure kettle 3, sampling detects; 8, after reaction terminates, logical condensate water is down to room temperature, and still is driven in release.
The temperature range of the work of the High Temperature High Pressure kettle 1 in the present invention is: room temperature ~ 400 DEG C, and working pressure range is: 10
3~ 3 × 10
7pa.
Embodiment 2
The one end adding air pipe passes into High Temperature High Pressure kettle 1, and the other end can connect an interface of threeway, and another two interfaces of threeway connect pressurized-gas source and reacting gas source through needle-valve respectively.
First stopple coupon 10 one end enters in buffering kettle 2, and the other end is split up into gas sample tube 5 and liquid sampling pipe 6 Liang Ge branch, also can adopt threeway realize gas sample tube 5 and liquid sampling pipe 6 separately.
Second stopple coupon 13 one end enters in buffering kettle 2, and the other end is split up into gas sample tube 11 and liquid sampling Guan12Liang Ge branch, also can adopt threeway realize gas sample tube 11 and liquid sampling pipe 12 separately.
Embodiment 3
Automatic control box 9 can adopt the control method of prior art and control circuit to realize.
Claims (4)
1. one kind has the high-temperature high-pressure reaction kettle of on-line period device, comprise the High Temperature High Pressure kettle (1) having liquid inlet opening and gas feed(raw material)inlet, High Temperature High Pressure kettle (1) heating outward, cooling and attemperator, and pressue device; It is characterized in that, structure cushions kettle (2) and normal temperature and pressure kettle (3) in addition; Between High Temperature High Pressure kettle (1) and buffering kettle (2), there is the first stopple coupon (10) to be communicated with, between buffering kettle (2) and normal temperature and pressure kettle (3), have the second stopple coupon (13) to be communicated with; Described the first stopple coupon (10), valve is equipped with in centre, one end is inserted in buffering kettle (2), the other end also connects gas sample tube (5) and liquid sampling pipe (6), gas sample is got at the top of opening in High Temperature High Pressure kettle (1) of gas sample tube (5), and liquid-like is got in the bottom of opening in High Temperature High Pressure kettle (1) of liquid sampling pipe (6); Described the second stopple coupon (13), valve is equipped with in centre, one end is inserted in normal temperature and pressure kettle (3), the other end also connects stopple coupon (11) and lower stopple coupon (12), the opening of upper stopple coupon (11) gets gas sample at the top of buffering kettle (2), and the opening of lower stopple coupon (12) gets liquid-like in the bottom of buffering kettle (2); Described normal temperature and pressure kettle (3), top has gas vent and is connected with checkout equipment, and bottom has liquid outlet to be connected with checkout equipment; Described pressue device, has and adds air pipe, pressurized-gas source and supercharge pump (7), and the one end adding air pipe passes in High Temperature High Pressure kettle (1), and the other end is connected pressurized-gas source through gas valve with supercharge pump (7); Unstrpped gas enters through valve and adds air pipe and enter in High Temperature High Pressure kettle (1) again.
2. the high-temperature high-pressure reaction kettle with on-line period device according to claim 1, is characterized in that, High Temperature High Pressure kettle (1) arranges electric mixer (4); Outside High Temperature High Pressure kettle (1), arrange vacuum pump (8), vacuum pump (8) communicates with in High Temperature High Pressure kettle (1) through gas valve.
3. the high-temperature high-pressure reaction kettle with on-line period device according to claim 1 and 2, is characterized in that, High Temperature High Pressure kettle (1) is equipped with rain glass, in heating, cooling and attemperator, temperature probe is housed; In buffering kettle (2), temperature sensor and pressure transducer are housed; Automatic control box (9) is had outside High Temperature High Pressure kettle (1), automatic control box (9) is built with on-line period control device, mixing control device, temperature control equipment, the pressure control device of High Temperature High Pressure kettle (1), vacuumize control device, and the display device of the temperature and pressure of buffering kettle (2).
4. the high-temperature high-pressure reaction kettle with on-line period device according to claim 1 and 2, is characterized in that, gas sample tube (5) and liquid sampling pipe (6) are respectively equipped with needle-valve; Upper stopple coupon (11) and lower stopple coupon (12) are respectively equipped with needle-valve.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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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| Application Number | Priority Date | Filing Date | Title |
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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 CN102773042A (en) | 2012-11-14 |
| CN102773042B true CN102773042B (en) | 2015-04-08 |
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Cited By (1)
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| CN105126702A (en) * | 2015-09-24 | 2015-12-09 | 东北大学 | High-pressure reaction kettle capable of online measuring potential of pressurizing wet-method system |
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| 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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- 2012-08-15 CN CN201210290826.7A patent/CN102773042B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN202284988U (en) * | 2011-10-10 | 2012-06-27 | 恒升化工（启东）有限公司 | Pressurized liquid sampling device |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105126702A (en) * | 2015-09-24 | 2015-12-09 | 东北大学 | High-pressure reaction kettle capable of online measuring potential of pressurizing wet-method system |
| CN105126702B (en) * | 2015-09-24 | 2017-09-05 | 东北大学 | It is a kind of can on-line measurement Pressure hydrometallurgical process system current potential autoclave |
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| CN102773042A (en) | 2012-11-14 |
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