阅读说明：本技术 一种内置换热式超临界二氧化碳分离方法及设备 (Built-in heat exchange type supercritical carbon dioxide separation method and equipment ) 是由 刘汉槎 徐继涛 伍淑华 刘粤华 陈羽豪 于 2020-12-31 设计创作，主要内容包括：本发明公开一种内置换热式超临界二氧化碳分离设备,包括分离釜壳体,分离釜壳体的中间位置设置有流体入口,流体入口的下方设置有换热盘管,换热盘管的上端设置有盘管进水口,换热盘管的下端设置有盘管出水口,换热盘管设置在分离釜壳体的内部,分离釜的上方设置有流体出口,流体出口与流体入口之间设置有捕沫过滤器,分离釜壳体的底部设置有物料出口,并公开相应的分离方法,本发明通过采用特殊的分离釜结构和专用分离工艺过程,实现CO2和溶质的高效的分离,提高回收CO2的纯度。是用于超临界CO2植物萃取、无水染色、纳米气凝胶干燥、塑料发泡等应用领域的工艺方法及设备。(The invention discloses a built-in heat exchange type supercritical carbon dioxide separation device, which comprises a separation kettle shell, wherein a fluid inlet is arranged at the middle position of the separation kettle shell, a heat exchange coil is arranged below the fluid inlet, a coil water inlet is arranged at the upper end of the heat exchange coil, a coil water outlet is arranged at the lower end of the heat exchange coil, the heat exchange coil is arranged in the separation kettle shell, a fluid outlet is arranged above the separation kettle, a foam catching filter is arranged between the fluid outlet and the fluid inlet, and a material outlet is arranged at the bottom of the separation kettle shell. Is a process method and equipment used in the application fields of supercritical CO2 plant extraction, anhydrous dyeing, nano aerogel drying, plastic foaming and the like.)

1. The utility model provides a built-in heat transfer formula supercritical carbon dioxide splitter, its characterized in that, including separation cauldron casing (4), the intermediate position of separation cauldron casing (4) is provided with fluid entry (5), the below of fluid entry (5) is provided with heat transfer coil (10), the upper end of heat transfer coil (10) is provided with coil water inlet (9), the lower extreme of heat transfer coil (10) is provided with coil water outlet (11), heat transfer coil (10) set up the inside of separation cauldron casing (4), the top of separation cauldron is provided with fluid outlet (2), fluid outlet (2) with be provided with between fluid entry (5) and catch foam filter (12), the bottom of separation cauldron casing (4) is provided with material export (8).

2. The apparatus for supercritical carbon dioxide separation with built-in heat exchange according to claim 1 is characterized by a guiding elbow at the fluid inlet (5), the upper end of the guiding elbow is arranged above the heat exchange coil (10), and the lower end of the guiding elbow extends to the bottom end position of the separation vessel shell (4).

3. The supercritical carbon dioxide separation equipment with built-in heat exchange according to claim 2 is characterized in that the top of the separation kettle shell (4) is provided with a quick-open end cover (1), and the fluid outlet (2) is arranged below the quick-open end cover (1).

4. The supercritical carbon dioxide separation equipment with built-in heat exchange type according to claim 3 is characterized in that the heat exchange coil (10) is spirally arranged on the inner wall of the separation kettle shell (4), the heat exchange coil (10) is made of carbon steel, and the wall thickness of the heat exchange coil (10) is 2.0 mm.

5. The supercritical carbon dioxide separation equipment with built-in heat exchange according to claim 1 is characterized in that the outer wall of the separation kettle shell (4) is provided with a support (3).

6. The supercritical carbon dioxide separation equipment with built-in heat exchange type according to claim 1, wherein the separation kettle shell (4) is provided with a first liquid level meter interface (6) corresponding to the position of the heat exchange coil (10), a first liquid level meter is arranged at the first liquid level meter interface (6), a second liquid level meter interface (7) is arranged below the separation kettle shell (4), and a second liquid level meter is arranged at the second liquid level meter interface (7).

7. The supercritical carbon dioxide separation method with built-in heat exchange according to claim 1 is characterized in that the inner wall of the separation kettle shell (4) is provided with a temperature sensor.

8. A method for separating supercritical carbon dioxide with built-in heat exchange, comprising the supercritical carbon dioxide separation equipment with built-in heat exchange of any one of claims 1 to 7, characterized by comprising the steps of:

s1, introducing the reaction fluid into the fluid inlet (5) and entering the bottom end of the reaction kettle shell along the guide elbow;

s2, controlling the temperature of water led into the heat exchange coil (10) according to the real-time temperature inside the reaction kettle shell detected by the temperature sensor, and realizing heat exchange between the heat exchange coil (10) and reaction fluid;

s3, heating and vaporizing liquid carbon dioxide in the reaction fluid, then ascending to enter an entrainment filter (12), filtering gaseous carbon dioxide by the entrainment filter (12), gathering and condensing fluid liquid, and then refluxing to the bottom end of the reaction kettle shell;

s4, discharging the gaseous carbon dioxide out of the separation kettle shell (4) through the fluid outlet (2), and discharging the reaction fluid into the next working procedure through the material outlet (8).

9. The method for separating supercritical carbon dioxide with built-in heat exchange according to claim 8, wherein the step S2 specifically includes that the heat exchange coil (10) can adjust the flow of hot water or cold water according to the real-time temperature fed back by the temperature sensor to achieve the effect of temperature increase or temperature decrease.

Technical Field

The invention relates to the technical field of fabric dyeing and finishing equipment, in particular to built-in heat exchange type supercritical carbon dioxide separation equipment and a built-in heat exchange type supercritical carbon dioxide separation method.

Background

The supercritical CO2 fluid technology can be widely applied to the industrial fields of plant extraction, nano aerogel drying, anhydrous dyeing, plastic foaming and the like due to high-efficiency solubility, reliability and safety. In the process of the supercritical CO2 fluid technology, the separation of CO2 is an important link. In the CO2 separation link, CO2 is gasified and separated from solute dissolved in supercritical CO2, so that CO2 is recovered and recycled. Meanwhile, the separated solute components are discharged from the lower part of the separation kettle. Depending on the field of application, the separated solutes are either collected as a product or discharged as a reject. In either case, CO2 is a purification process for CO 2. It is clear that the more complete the separation, the higher the purity of the CO2 recovered for recycle. The purity of CO2 at this time directly affects the dissolving capacity when CO2 is recycled, and thus directly affects the production efficiency.

Disclosure of Invention

Aiming at the problems, the invention provides built-in heat exchange type supercritical carbon dioxide separation equipment and a built-in heat exchange type supercritical carbon dioxide separation method, a separation kettle structure with a built-in heat exchange device is adopted, and through a mass transfer process with backflow, the defects that a common cavity type separation kettle is not thoroughly analyzed and CO2 is not thoroughly separated and purified due to entrainment are avoided, and a CO2 purification process with higher precision is realized.

The invention provides a built-in heat exchange type supercritical carbon dioxide separation device which comprises a separation kettle shell, wherein a fluid inlet is formed in the middle of the separation kettle shell, a heat exchange coil is arranged below the fluid inlet, a coil water inlet is formed in the upper end of the heat exchange coil, a coil water outlet is formed in the lower end of the heat exchange coil, the heat exchange coil is arranged inside the separation kettle shell, a fluid outlet is formed above the separation kettle, a foam catching filter is arranged between the fluid outlet and the fluid inlet, and a material outlet is formed in the bottom of the separation kettle shell.

In a further improvement, a guide elbow is arranged at the fluid inlet, the upper end of the guide elbow is arranged above the heat exchange coil, and the lower end of the guide elbow extends to the bottom end of the separation kettle shell.

The further improvement lies in that the top of the separation kettle shell is provided with a quick-opening end cover, and the fluid outlet is arranged below the quick-opening end cover.

The further improvement lies in that heat exchange coil is the heliciform setting and is in on the inner wall of separation cauldron casing, just the material that heat exchange coil adopted is the carbon steel, heat exchange coil's wall thickness is 2.0 mm.

The further improvement lies in that a support is arranged on the outer wall of the separation kettle shell.

The improved separation kettle is characterized in that the separation kettle shell corresponds to a first liquid level meter interface is arranged at the position of the heat exchange coil, a first liquid level meter is arranged at the first liquid level meter interface, a second liquid level meter interface is arranged below the separation kettle shell, and a second liquid level meter is arranged at the second liquid level meter interface.

The further improvement lies in that a temperature sensor is arranged on the inner wall of the separation kettle shell.

The second aspect of the invention provides a built-in heat exchange type supercritical carbon dioxide separation method, which comprises the following steps:

s1, introducing the reaction fluid into the fluid inlet and entering the bottom end of the reaction kettle shell along the guide elbow;

s2, controlling the temperature of water entering the heat exchange coil according to the real-time temperature inside the reaction kettle shell detected by the temperature sensor, and realizing heat exchange between the heat exchange coil and reaction fluid;

s3, heating and vaporizing liquid carbon dioxide in the reaction fluid, then ascending to enter an entrainment filter, filtering gaseous carbon dioxide by the entrainment filter, gathering and condensing the fluid liquid, and then refluxing to the bottom end of the reaction kettle shell;

and S4, discharging the gaseous carbon dioxide out of the separation kettle shell through the fluid outlet, and discharging the reaction fluid into the next working procedure through the material outlet.

The further improvement is that step S2 specifically includes that the heat exchange coil can adjust the hot water or cold water introduced according to the real-time temperature fed back by the temperature sensor, so as to achieve the effect of temperature rise or temperature reduction.

Compared with the prior art, the invention has the beneficial effects that:

the process method and the equipment structure can effectively improve the effect that the solute dissolved in the supercritical state CO2 is thoroughly separated in the CO2 fluid technology, so that the CO2 can be recovered and recycled. In the plant extraction application, the complete separation operation can be carried out, and the plant effective components with higher purity can be obtained. The separation of residual dye can be improved in the anhydrous dyeing application; in the application of the nano aerogel, the separation degree of alcohol in CO2 can be improved, CO2 can be further purified, the high solubility of CO2 in the drying process is kept, and the drying efficiency is greatly improved.

Drawings

The drawings are for illustrative purposes only and are not to be construed as limiting the patent; for the purpose of better illustrating the embodiments, certain features of the drawings may be omitted, enlarged or reduced, and do not represent the size of an actual product; it will be understood by those skilled in the art that certain well-known structures in the drawings and descriptions thereof may be omitted.

FIG. 1 is a schematic overall structure diagram of an embodiment of the present invention;

wherein: 1. a quick-open end cap; 2. a fluid outlet; 3. a support; 4. separating the kettle shell; 5. a fluid inlet; 6. a first level meter interface; 7. a second level gauge interface; 8. a material outlet; 9. a coil pipe water inlet; 10. a heat exchange coil; 11. a water outlet of the coil pipe; 12. a foam trapping filter.

Detailed Description

In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted" and "connected" are to be interpreted broadly, e.g., as being either fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, so to speak, as communicating between the two elements. The specific meaning of the above terms in the present invention can be understood in specific cases to those skilled in the art. The technical solution of the present invention is further described below with reference to the accompanying drawings and examples.

Referring to fig. 1, a built-in heat exchange type supercritical carbon dioxide separation device comprises a separation kettle shell 4, a fluid inlet 5 is arranged at the middle position of the separation kettle shell 4, a heat exchange coil 10 is arranged below the fluid inlet 5, a coil water inlet 9 is arranged at the upper end of the heat exchange coil 10, a coil water outlet 11 is arranged at the lower end of the heat exchange coil 10, the heat exchange coil 10 is arranged inside the separation kettle shell 4, a fluid outlet 2 is arranged above the separation kettle, a foam catching filter 12 is arranged between the fluid outlet 2 and the fluid inlet 5, and a material outlet 8 is arranged at the bottom of the separation kettle shell 4.

In a preferred embodiment of the present invention, a guiding elbow is disposed at the fluid inlet 5, the upper end of the guiding elbow is disposed above the heat exchange coil 10, and the lower end of the guiding elbow extends to the bottom end position of the separation tank shell 4.

As a preferred embodiment of the invention, the top of the separation kettle shell 4 is provided with a quick-open end cover 1, and the fluid outlet 2 is arranged below the quick-open end cover 1.

As a preferred embodiment of the present invention, the heat exchange coil 10 is spirally disposed on the inner wall of the separation kettle shell 4, the heat exchange coil 10 is made of carbon steel, and the wall thickness of the heat exchange coil 10 is 2.0 mm.

In a preferred embodiment of the present invention, the outer wall of the separation tank housing 4 is provided with a support 3.

As a preferred embodiment of the present invention, a first liquid level meter interface 6 is disposed at a position of the separation kettle shell 4 corresponding to the heat exchange coil 10, a first liquid level meter is disposed at the first liquid level meter interface 6, a second liquid level meter interface 7 is disposed below the separation kettle shell 4, and a second liquid level meter is disposed at the second liquid level meter interface 7.

As a preferred embodiment of the present invention, a temperature sensor is disposed on the inner wall of the separation tank housing 4.

The invention relates to a process and equipment for separating and purifying CO2 in a supercritical CO2 fluid technology, wherein a supercritical CO2 fluid is dissolved in an extraction kettle of a previous process and then enters a separation kettle, CO2 is separated from a solute, CO2 enters a subsequent process for condensation and liquefaction for recycling, the separation equipment is a separation kettle with a built-in heat exchanger, the heat exchanger in the separation kettle realizes heating or cooling operation, and meanwhile, the top condensed and refluxed liquid can improve the purity of CO2 separation, and a built-in heat exchange type supercritical carbon dioxide separation method is also provided, and comprises the following steps:

s1, introducing the reaction fluid into the fluid inlet 5 and entering the bottom end of the reaction kettle shell along the guide elbow;

s2, controlling the temperature of water led into the heat exchange coil 10 according to the real-time temperature inside the reaction kettle shell detected by the temperature sensor, and realizing heat exchange between the heat exchange coil 10 and reaction fluid;

s3, heating and vaporizing the liquid carbon dioxide in the reaction fluid, then ascending to enter the foam catching filter 12, filtering gaseous carbon dioxide by the foam catching filter 12, gathering and condensing the fluid liquid, and then refluxing to the bottom end of the reaction kettle shell;

s4, discharging the gaseous carbon dioxide out of the separation kettle shell 4 through the fluid outlet 2, and discharging the reaction fluid into the next working procedure through the material outlet 8.

Specifically, CO2 fluid which is discharged from an outlet of the extraction kettle and subjected to pressure reduction enters the separation kettle through a fluid inlet 5, and the inlet impact can be buffered due to the fact that the bent pipe is guided to enter under liquid, so that entrainment can be reduced; the decompressed CO2 becomes a gas state, the material components dissolved in the CO2 are separated from the CO2, the gas state CO2 is settled at the bottom of the reaction kettle and can be discharged out of the separation kettle through a material outlet 8, the gaseous CO2 is discharged out of the separation kettle through a fluid outlet 2 and enters a subsequent condensation process, a built-in heat exchange coil 10 is a heat exchange component, hot water or cold water is introduced into the tube, and the heating and cooling operation can be carried out according to the process requirement; the liquid level meter interface is used for connecting a liquid level meter to monitor the reaction liquid level in the separation kettle, so that the reaction liquid level is kept at the level required by the process; the mist trapping filter 12 on the top of the kettle is used for intercepting part of impurities carried by mist, the reflux of liquid can adjust the solubility, the further analysis operation is facilitated, and the purification of CO2 is improved.

As a preferred embodiment of the present invention, the step S2 specifically includes that the heat exchanging coil 10 can adjust the temperature of the hot water or the cold water according to the real-time temperature fed back by the temperature sensor, so as to achieve the effect of temperature increase or temperature decrease.

Compared with the prior art, the invention has the beneficial effects that:

the process method and the equipment structure can effectively improve the effect that the solute dissolved in the supercritical state CO2 is thoroughly separated in the CO2 fluid technology, so that the CO2 can be recovered and recycled. In the plant extraction application, the complete separation operation can be carried out, and the plant effective components with higher purity can be obtained. The separation of residual dye can be improved in the anhydrous dyeing application; in the application of the nano aerogel, the separation degree of alcohol in CO2 can be improved, CO2 can be further purified, the high solubility of CO2 in the drying process is kept, and the drying efficiency is greatly improved.

In the drawings, the positional relationship is described for illustrative purposes only and is not to be construed as limiting the present patent; it should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.