CN107036393B - Device and process for producing 5N-grade high-purity propane by adopting double-tower continuous rectification - Google Patents
Device and process for producing 5N-grade high-purity propane by adopting double-tower continuous rectification Download PDFInfo
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- CN107036393B CN107036393B CN201710417335.7A CN201710417335A CN107036393B CN 107036393 B CN107036393 B CN 107036393B CN 201710417335 A CN201710417335 A CN 201710417335A CN 107036393 B CN107036393 B CN 107036393B
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/08—Separating gaseous impurities from gases or gaseous mixtures or from liquefied gases or liquefied gaseous mixtures
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
- F25J3/0228—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream
- F25J3/0242—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream separation of CnHm with 3 carbon atoms or more
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2200/00—Processes or apparatus using separation by rectification
- F25J2200/04—Processes or apparatus using separation by rectification in a dual pressure main column system
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2200/00—Processes or apparatus using separation by rectification
- F25J2200/04—Processes or apparatus using separation by rectification in a dual pressure main column system
- F25J2200/06—Processes or apparatus using separation by rectification in a dual pressure main column system in a classical double column flow-sheet, i.e. with thermal coupling by a main reboiler-condenser in the bottom of low pressure respectively top of high pressure column
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2200/00—Processes or apparatus using separation by rectification
- F25J2200/40—Features relating to the provision of boil-up in the bottom of a column
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2200/00—Processes or apparatus using separation by rectification
- F25J2200/50—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2200/00—Processes or apparatus using separation by rectification
- F25J2200/72—Refluxing the column with at least a part of the totally condensed overhead gas
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2200/00—Processes or apparatus using separation by rectification
- F25J2200/74—Refluxing the column with at least a part of the partially condensed overhead gas
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2215/00—Processes characterised by the type or other details of the product stream
- F25J2215/64—Propane or propylene
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2270/00—Refrigeration techniques used
- F25J2270/12—External refrigeration with liquid vaporising loop
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Abstract
The invention belongs to a device and a production process for producing 5N-grade high-purity propane by adopting double-tower continuous rectification; the device comprises a raw material liquid storage tank and a product storage tank, wherein the raw material liquid storage tank sequentially passes through a first raw material inlet of a first heat exchanger, a first raw material outlet of the first heat exchanger, a first raw material inlet of a first rectifying tower, a gas-phase outlet of the first rectifying tower, a first raw material inlet of a second heat exchanger, a first raw material outlet of the second heat exchanger, a raw material inlet of a gas-liquid separator, a liquid-phase outlet of the gas-liquid separator, a second raw material inlet of the first rectifying tower, a liquid-phase outlet of the first rectifying tower, a first raw material of the second rectifying tower, a gas-phase outlet of the second rectifying tower, a second raw material inlet of the second heat exchanger and a second raw material outlet of the second heat exchanger to be connected with a first tee joint, and a third end of the first tee joint is connected with the product storage tank through a seventh regulating valve; the method has the advantages that the purity of the propane product is high, the requirement of microelectronic and optoelectronic elements on propane can be met, the yield is high, and the method can be suitable for large-scale industrial production.
Description
Technical Field
The invention belongs to the technical field of producing 5N-grade high-purity propane, and particularly relates to a device and a production process for producing 5N-grade high-purity propane by adopting double-tower continuous rectification.
Background
The high-purity propane is a gas with wide application, is an important component gas in gas distribution production, is also an important production raw material of optoelectronic elements, has larger and larger demand with the development of optoelectronic industry in China, and has good market prospect. The industrial propane with the purity of 85 percent which is conveniently purchased on the market is used as the raw material, so that the raw material cost is greatly saved.
Some of the processes in large-scale industrial processes can produce high purity propane, and several techniques are now introduced that are suitable for small-batch production of high purity propane.
1. Large scale chromatography; also known as preparative chromatography. The principle is that gas-liquid or gas-solid chromatography is carried out, a certain volume of raw gas is injected into carrier gas flow by a sample injector, namely the raw gas is taken away by carrier gas, is adsorbed and desorbed by a chromatographic separation column and is separated into a plurality of chromatographic peaks, an analysis controller is used for observing the separation process and determining the normal operation position of an automatic valve, the components to be obtained are respectively cut out, the components are sent to a cold trap to remove impurity peaks, and then the gas sent to the cold trap is separated from the carrier gas by a freezing or condensing method, so that high-purity propane is obtained.
2. A chemical absorption-adsorption method; the basic idea of the process is to remove propylene impurities with high content and similar physical properties to propane by a chemical absorption method, remove residual hydrocarbon impurities such as propylene and the like by an adsorption method, and remove low boiling point impurities such as nitrogen, oxygen, methane, hydrogen and the like by a condensation method to prepare pure propane. Adsorptive separation is achieved by separating different components of a mixture according to their adsorption characteristics on the same solid substance (adsorbent).
3. Adsorption-condensation method; the principle is that the adsorption-condensation separation technology is used to extract high-purity propane from liquefied gas. The components of the mixture are separated from each other by the ability of the surface energy of the adsorbent to selectively adsorb certain components from the fluid. The adsorbent of a certain type is selected as a purifying agent. It has the ability to preferentially adsorb polar molecules and unsaturated hydrocarbon molecules. The raw material is adsorbed to remove hydrocarbon impurities such as propylene, isobutane and the like, and low-boiling-point impurities such as nitrogen, oxygen and the like are separated and removed by a condensation method, so that high-purity propane of 99.995 percent can be obtained.
Disclosure of Invention
The invention aims to overcome the defects of complex equipment, large investment, large energy consumption of low-temperature condensation and rectification, low thermodynamic efficiency and low purity of high-purity propane in the traditional process, and provides a device and a production process for producing 5N-grade high-purity propane by adopting double-tower continuous rectification, wherein mixed gas of propane and ethane is firstly used as a heat source to provide heat for a reboiler at the bottom of a rectifying tower as the heat source, and then the mixed gas is condensed into liquid and is subjected to throttling and pressure reduction to provide cold energy for a condenser at the top of the rectifying tower, so that the comprehensive utilization of energy is realized, and the energy utilization efficiency of the system is improved.
The invention realizes the purpose through the following technical scheme: the system comprises a raw material liquid storage tank, a product storage tank, a refrigerating device and a waste gas furnace, wherein the raw material liquid storage tank is connected with a first raw material inlet of a first heat exchanger through a pipeline, a first raw material outlet of the first heat exchanger is connected with a first raw material inlet of a first rectifying tower through a first regulating valve, a gas phase outlet at the top of the first rectifying tower is connected with a first raw material gas inlet of a second heat exchanger through a pipeline, a first raw material outlet of the second heat exchanger is connected with a raw material inlet of a gas-liquid separator through a pipeline, a liquid phase outlet of the gas-liquid separator is connected with a second raw material inlet of the first rectifying tower through a pipeline, a tower bottom liquid phase outlet of the first rectifying tower is connected with a first raw material inlet of a second rectifying tower through a third regulating valve, a tower top gas phase outlet of the second rectifying tower is connected with a second raw material gas inlet of the second heat exchanger through a pipeline, a second raw material outlet of the second heat exchanger is connected with a first tee joint through a fourth regulating valve, a third tee joint of the first tee joint is connected with a product storage tank, a second raw material outlet of the second rectifying tower bottom of the second rectifying tower is connected with a waste gas-liquid outlet of the first rectifying tower through a third regulating valve, and a waste gas-liquid outlet of the first rectifying tower are connected with a raw material inlet of the ninth heat exchanger through a third regulating valve, and a waste gas-liquid heat exchanger, and a waste gas-waste gas outlet of the ninth raw material inlet of the ninth heat exchanger; an outlet of the refrigerating device is connected with a second tee joint, a second end of the second tee joint is connected with a first mixed gas inlet of the first heat exchanger through a pipeline, and a first mixed gas outlet of the first heat exchanger is connected with a first end of a third tee joint through a fifth regulating valve and a reboiler of the second rectifying tower; the third end of the second tee joint is connected with the second end of the third tee joint through a second regulating valve and a reboiler of the first rectifying tower; the third end of the third tee joint is connected with a mixed liquid inlet of the second heat exchanger through a sixth regulating valve, a mixed liquid outlet of the second heat exchanger is connected with a second mixed gas inlet of the first heat exchanger through a pipeline, and a second mixed gas outlet of the first heat exchanger is connected with an inlet of the refrigerating device through a tenth regulating valve.
A production process of a device for producing 5N-grade high-purity propane by adopting double-tower continuous rectification comprises the following steps:
the method comprises the following steps: the raw material liquid in the raw material liquid storage tank enters a first raw material liquid inlet of a first rectifying tower after passing through a first raw material inlet of a first heat exchanger, a first raw material outlet of the first heat exchanger and a first regulating valve, and the raw material liquid is: 85# industrial propane, wherein the raw material liquid comprises the following components: propane, methane, ethane, carbon dioxide, n-butane, isobutane, water, ethylene, propylene, dimethyl ether, oxygen, nitrogen; the temperature of the feed solution is 40 ℃, the pressure is 2.2MPA (absolute pressure), the gas phase fraction is 0, the mole fraction of propane is 85%, the temperature of the feed solution after passing through the first heat exchanger is 10 ℃, and the temperature of the feed solution after passing through the first regulating valve is as follows: -30 ℃;
step two: enabling the raw material liquid passing through a first raw material liquid inlet of the first rectifying tower in the first step to enter the first rectifying tower for rectification and purification, enabling a gas phase after rectification and purification to enter a second heat exchanger for heat exchange and condensation through a gas phase outlet at the top of the first rectifying tower and a first raw material gas inlet of the second heat exchanger, enabling a raw material gas after heat exchange and condensation to enter a gas-liquid separator through a first raw material outlet of the second heat exchanger for gas-liquid separation, enabling a liquid phase communication to flow back into the first rectifying tower through a liquid phase outlet of the gas-liquid separator and a second raw material inlet of the first rectifying tower, enabling a gas phase communication to enter the first heat exchanger through a gas phase outlet of the gas-liquid separator and a second raw material inlet of the first heat exchanger for cold recovery, and enabling tail gas after cold recovery to be conveyed into the waste gas furnace through a second raw material outlet of the first heat exchanger and an eighth regulating valve for treatment; the temperature of the raw material gas at the gas phase outlet at the top of the first rectifying tower is as follows: -35.6 ℃, and the temperature of the feed gas at the first feed outlet of the second heat exchanger is: -37 ℃ and the tail gas temperature at the second feed outlet of the first heat exchanger is: 1 deg.C;
step three: feeding the raw material liquid at the tower bottom liquid phase outlet of the first rectifying tower in the second step into a second rectifying tower through a third regulating valve and a first raw material inlet of the second rectifying tower for rectification, feeding the rectified liquid phase into a first heat exchanger through a tower bottom liquid phase outlet of the second rectifying tower and a third raw material inlet of the first heat exchanger for heat exchange, recovering cold energy, and feeding the tail gas after cold energy recovery into a waste gas furnace through a third raw material outlet of the first heat exchanger and a ninth regulating valve; the rectified gas phase is divided into two streams through a gas phase outlet at the top of the second rectifying tower, a second raw material gas inlet of the second heat exchanger and a second raw material outlet of the second heat exchanger, one stream enters the second rectifying tower through a fourth regulating valve and a second raw material inlet of the second rectifying tower to flow back, and the other stream enters a product storage tank through a seventh regulating valve; the temperature of the raw material liquid entering the first raw material inlet of the second rectifying tower is as follows: -26 ℃, pressure: 0.18MPa (absolute pressure); the temperature of the raw material gas at the gas phase outlet at the top of the second rectifying tower is as follows: -36 ℃ and the product temperature at the second feed outlet of the second heat exchanger is: -37 ℃, pressure: 0.13MPa (absolute pressure), gas phase fraction of 0, and mole fraction of propane of 99.9994%;
step four: in the process of refrigeration cycle, a refrigerant in the refrigeration device is divided into two streams, wherein one stream is subjected to heat exchange with a first mixed gas inlet of a first heat exchanger and precooled to 10 ℃, then passes through a first mixed gas outlet of the first heat exchanger 2, a fifth regulating valve and a reboiler of a second rectifying tower and then enters a third tee, the other stream passes through a second regulating valve and the reboiler of the first rectifying tower and then enters the third tee, then the two mixed liquids are mixed, throttled and depressurized by a sixth regulating valve and then enter a second heat exchanger through a mixed liquid inlet of the second heat exchanger to provide cold energy for the mixed liquids, so that the gas at the top of the first rectifying tower and the second rectifying tower is condensed and refluxed, the gasified mixed gas enters a second heat exchanger through a third outlet of the second heat exchanger and a second mixed gas inlet of the first heat exchanger, and the cold energy is recycled in the inlet of the refrigeration device through a second mixed gas outlet of the first heat exchanger and a tenth regulating valve after being recycled in the second heat exchanger.
The invention has the following advantages:
1. the purity of the propane produced by the method reaches 99.9994 percent, the quality of the propane can completely meet the requirements of microelectronic and optoelectronic elements on the propane, the propane can be continuously produced, the production capacity is large, large-scale industrial production can be completely carried out, the blank of domestic high-purity propane industrial production is filled, and the method has good economic benefit and social benefit.
2. The rectification system adopts a double-tower rectification technology, the mixed gas is skillfully provided with heat for a reboiler at the tower bottom by adopting the mixed gas of propane and ethane as the refrigerant, the temperature is reduced, and then throttling depressurization is carried out to provide cold energy for a condenser shared by the tower top, so that the energy transfer is realized, the energy consumption is reduced, the utilization efficiency of the energy is greatly improved, the refrigeration flow is greatly simplified, the safety coefficient in the production is also improved, and the rectification system has revolutionary progress compared with the traditional process.
3. In the production process, double-tower rectification is adopted without additional operation units, and compared with an adsorption rectification method, the method has the advantages of low investment cost of production equipment, low energy consumption and large profit margin of products.
Drawings
FIG. 1 is a schematic structural diagram of the present invention.
Fig. 2 is a schematic structural diagram of a first heat exchanger according to the present invention.
Detailed Description
In order to more clearly understand the technical features, objects, and effects of the present invention, embodiments of the present invention will now be described with reference to the accompanying drawings, in which like reference numerals refer to like parts throughout. For the sake of simplicity, only the parts relevant to the invention are schematically shown in the drawings, and they do not represent the actual structure as a product.
As shown in figures 1 and 2, the invention relates to a device and a production process for producing 5N-grade high-purity propane by adopting double-tower continuous rectification, the structure of the device comprises a raw material liquid storage tank 1, a product storage tank 48, a refrigerating device 50 and a waste gas furnace 51, wherein the raw material liquid storage tank 1 is connected with a first raw material inlet 17 of a first heat exchanger 2 through a pipeline, a first raw material outlet 24 of the first heat exchanger 2 is connected with a first raw material inlet 27 of a first rectifying tower 4 through a first regulating valve 3, a gas phase outlet 28 at the top of the first rectifying tower 4 is connected with a first raw material gas inlet 34 of a second heat exchanger 6 through a pipeline, a first raw material outlet 38 of the second heat exchanger 6 is connected with a raw material inlet 39 of a gas-liquid separator 7 through a pipeline, a liquid phase outlet 41 of the gas-liquid separator 7 is connected with a second raw material inlet 29 of the first rectifying tower 4 through a pipeline, a tower bottom liquid phase outlet 31 of the first rectifying tower 4 is connected with a first raw material inlet 46 of the second rectifying tower 9 through a third regulating valve 5, a tower top gas phase outlet 42 of the second rectifying tower 9 is connected with a second raw material gas inlet 36 of the second heat exchanger 6 through a pipeline, a second raw material outlet 33 of the second heat exchanger 6 is connected with a first tee joint 49, a second end of the first tee joint 49 is connected with a second raw material inlet 47 of the second rectifying tower 9 through a fourth regulating valve 8, a third end of the first tee joint 49 is connected with a product storage tank 48 through a seventh regulating valve 10, a tower bottom liquid phase outlet 44 of the second rectifying tower 9 is connected with a third raw material inlet 18 of the first heat exchanger 2 through a pipeline, a third raw material outlet 23 of the first heat exchanger 2 is connected with a waste gas furnace 51 through a ninth regulating valve 12, a gas phase outlet 40 of the gas-liquid separator 7 is connected with a second raw material inlet 19 of the first heat exchanger 2 through a pipeline, and a second raw material outlet 22 of the first heat exchanger 2 is connected with a waste gas furnace 51 through an eighth regulating valve 11; an outlet of the refrigerating device 50 is connected with a second tee joint 32, a second end of the second tee joint 32 is connected with a first mixed gas inlet 20 of the first heat exchanger 2 through a pipeline, and a first mixed gas outlet 25 of the first heat exchanger 2 is connected with a first end of a third tee joint 43 through a fifth regulating valve 14 and a reboiler 45 of the second rectifying tower 9; the third end of the second tee joint 32 is connected with the second end of the third tee joint 43 through a second regulating valve 13 and a reboiler 30 of the first rectifying tower 4; the third end of the third tee 43 is connected with the mixed liquid inlet 37 of the second heat exchanger 6 through the sixth regulating valve 15, the mixed liquid outlet 35 of the second heat exchanger 6 is connected with the second mixed gas inlet 26 of the first heat exchanger 2 through a pipeline, and the second mixed gas outlet 21 of the first heat exchanger 2 is connected with the inlet of the refrigerating device 50 through the tenth regulating valve 16.
A production process of a device for producing 5N-grade high-purity propane by adopting double-tower continuous rectification comprises the following steps:
the method comprises the following steps: the raw material liquid in the raw material liquid storage tank 1 enters a first raw material liquid inlet 27 of the first rectifying tower 4 after passing through a first raw material inlet 17 of the first heat exchanger 2, a first raw material outlet 24 of the first heat exchanger 2 and the first regulating valve 3, and the raw material liquid is: 85# industrial propane, wherein the raw material liquid comprises the following components: propane, methane, ethane, carbon dioxide, n-butane, isobutane, water, ethylene, propylene, dimethyl ether, oxygen, nitrogen; the temperature of the raw material liquid is 40 ℃, the pressure is 2.2MPA (absolute pressure), the gas phase fraction is 0, the mole fraction of propane is 85%, the temperature of the raw material liquid after passing through the first heat exchanger 2 is 10 ℃, and the temperature of the raw material liquid after passing through the first regulating valve 3 is as follows: -30 ℃;
step two: the raw material liquid passing through the first raw material liquid inlet 27 of the first rectifying tower 4 in the first step enters the first rectifying tower 4 for rectification and purification, the rectified and purified gas phase enters the second heat exchanger 6 for heat exchange and condensation through the gas phase outlet 28 at the top of the first rectifying tower 4 and the first raw material gas inlet 34 of the second heat exchanger 6, the raw material gas after heat exchange and condensation enters the gas-liquid separator 7 through the first raw material outlet 38 of the second heat exchanger 6 for gas-liquid separation, the liquid phase flows back to the first rectifying tower 4 through the liquid phase outlet 41 of the gas-liquid separator 7 and the second raw material inlet 29 of the first rectifying tower 4, the gas phase flows back to the first heat exchanger 2 through the gas phase outlet 40 of the gas-liquid separator 7 and the second raw material inlet 19 of the first heat exchanger 2 for cold recovery, and the tail gas after cold recovery is conveyed to the waste gas furnace 51 through the second raw material outlet 22 of the first heat exchanger 2 and the eighth regulating valve 11 for treatment; the temperature of the raw material gas at the gas phase outlet 28 at the top of the first rectifying tower 4 is as follows: -35.6 ℃ and the feed gas temperature at the first feed outlet 38 of the second heat exchanger 6 is: -37 ℃ and the tail gas temperature at the second feed outlet 22 of the first heat exchanger 2 is: 1 deg.C;
step three: raw material liquid at the tower bottom liquid phase outlet 31 of the first rectifying tower 4 in the second step enters the second rectifying tower 9 through the third regulating valve 5 and the first raw material inlet 46 of the second rectifying tower 9 for rectification, the rectified liquid phase enters the first heat exchanger 2 through the tower bottom liquid phase outlet 44 of the second rectifying tower 9 and the third raw material inlet 18 of the first heat exchanger 2 for heat exchange and then cold energy is recovered, and tail gas after cold energy recovery enters the waste gas furnace 51 through the third raw material outlet 23 of the first heat exchanger 2 and the ninth regulating valve 12; the rectified gas phase is divided into two parts after passing through a gas phase outlet 42 at the top of the second rectifying tower 9, a second raw material gas inlet 36 of the second heat exchanger 6 and a second raw material outlet 33 of the second heat exchanger 6, one part enters the second rectifying tower 9 through a fourth regulating valve 8 and a second raw material inlet 47 of the second rectifying tower 9 for reflux, and the other part enters a product storage tank 48 through a seventh regulating valve 10; the temperature of the raw material liquid entering the first raw material inlet 46 of the second rectifying tower 9 is as follows: -26 ℃, pressure: 0.18MPa (absolute pressure); the temperature of the raw material gas at the top gas phase outlet 42 of the second rectification tower 9 is as follows: -36 ℃ and the product temperature at the second feed outlet 33 of the second heat exchanger 6 is: -37 ℃, pressure: 0.13MPa (absolute pressure), gas phase fraction of 0, and mole fraction of propane of 99.9994%;
step four: in the process of refrigeration cycle, a refrigerant in the refrigeration device 50 is divided into two streams, wherein one stream of the refrigerant exchanges heat with a first mixed gas inlet 20 of the first heat exchanger 2 and is precooled to 10 ℃, then enters a third tee 43 after passing through a first mixed gas outlet 25 of the first heat exchanger 2, a fifth regulating valve 14 and a reboiler 45 of the second rectifying tower 9, the other stream of the refrigerant enters the third tee 43 after passing through a second regulating valve 13 and a reboiler 30 of the first rectifying tower 4, then the two streams of mixed liquid are mixed and are subjected to throttling and depressurization by a sixth regulating valve 15, the mixed liquid enters the second heat exchanger 6 through a mixed liquid inlet 37 of the second heat exchanger 6 to provide cold energy for the mixed liquid, so that the overhead gas of the first rectifying tower 4 and the second rectifying tower 9 is condensed and refluxed, the gasified mixed gas enters the second heat exchanger 6 through a third outlet 35 of the second heat exchanger 6 and a second mixed gas inlet 26 of the first heat exchanger 2, and the gasified mixed gas enters the second heat exchanger 6 through a second mixed gas outlet 21 of the first heat exchanger 2 and a tenth regulating valve 16 after the cold energy is recovered in the second heat exchanger 6 to be recycled for refrigeration by the refrigeration device 50.
The method can be suitable for industrial mass production, and is mainly characterized by low energy consumption, high product quality, 1000 KW/ton energy consumption, and product quality being improved to 99.999% electronic grade, wherein the adopted raw material is industrial grade ethane, and the industrial grade product is deeply purified and has lower energy consumption comparable to that of the traditional propane production process; compared with the traditional rectification, the invention optimizes the rectification process, improves the utilization efficiency of the refrigeration capacity of the rectification (compared with the traditional rectification and refrigeration), and reduces the energy consumption by about 8 to 10 percent.
The present invention will now be further illustrated with reference to examples in order to explain the present invention in more detail. The specific embodiment is as follows:
example one
A device for producing 5N-level high-purity propane by adopting double-tower continuous rectification comprises a raw material liquid storage tank 1, a product storage tank 48, a refrigerating device 50 and a waste gas furnace 51, wherein the raw material liquid storage tank 1 is connected with a first raw material inlet 17 of a first heat exchanger 2 through a pipeline, a first raw material outlet 24 of the first heat exchanger 2 is connected with a first raw material inlet 27 of the first rectifying tower 4 through a first regulating valve 3, a gas-phase outlet 28 at the top of the first rectifying tower 4 is connected with a first raw material gas inlet 34 of a second heat exchanger 6 through a pipeline, a first raw material outlet 38 of the second heat exchanger 6 is connected with a raw material inlet 39 of a gas-liquid separator 7 through a pipeline, a liquid-phase outlet 41 of the gas-liquid separator 7 is connected with a second raw material inlet 29 of the first rectifying tower 4 through a pipeline, a tower bottom liquid-phase outlet 31 of the first rectifying tower 4 is connected with a first raw material inlet 46 of the second rectifying tower 9 through a third regulating valve 5, a tower top gas phase outlet 42 of the second rectifying tower 9 is connected with a second raw material gas inlet 36 of the second heat exchanger 6 through a pipeline, a second raw material outlet 33 of the second heat exchanger 6 is connected with a first tee 49, a second end of the first tee 49 is connected with a second raw material inlet 47 of the second rectifying tower 9 through a fourth regulating valve 8, a third end of the first tee 49 is connected with a product storage tank 48 through a seventh regulating valve 10, a tower bottom liquid phase outlet 44 of the second rectifying tower 9 is connected with a third raw material inlet 18 of the first heat exchanger 2 through a pipeline, a third raw material outlet 23 of the first heat exchanger 2 is connected with a waste gas furnace 51 through a ninth regulating valve 12, a gas phase outlet 40 of the gas-liquid separator 7 is connected with a second raw material inlet 19 of the first heat exchanger 2 through a pipeline, and a second raw material outlet 22 of the first heat exchanger 2 is connected with the waste gas furnace 51 through an eighth regulating valve 11; an outlet of the refrigerating device 50 is connected with a second tee joint 32, a second end of the second tee joint 32 is connected with a first mixed gas inlet 20 of the first heat exchanger 2 through a pipeline, and a first mixed gas outlet 25 of the first heat exchanger 2 is connected with a first end of a third tee joint 43 through a fifth regulating valve 14 and a reboiler 45 of the second rectifying tower 9; the third end of the second tee 32 is connected with the second end of the third tee 43 through a second regulating valve 13 and a reboiler 30 of the first rectifying tower 4; the third end of the third tee joint 43 is connected with the mixed liquid inlet 37 of the second heat exchanger 6 through the sixth regulating valve 15, the mixed liquid outlet 35 of the second heat exchanger 6 is connected with the second mixed gas inlet 26 of the first heat exchanger 2 through a pipeline, and the second mixed gas outlet 21 of the first heat exchanger 2 is connected with the inlet of the refrigerating device 50 through the tenth regulating valve 16.
A production process of a device for producing 5N-grade high-purity propane by adopting double-tower continuous rectification comprises the following steps:
the method comprises the following steps: the raw material liquid in the raw material liquid storage tank 1 enters a first raw material liquid inlet 27 of the first rectifying tower 4 after passing through a first raw material inlet 17 of the first heat exchanger 2, a first raw material outlet 24 of the first heat exchanger 2 and the first regulating valve 3, and the raw material liquid is: 85# industrial propane, wherein the raw material liquid comprises the following components: propane, methane, ethane, carbon dioxide, n-butane, isobutane, water, ethylene, propylene, dimethyl ether, oxygen, nitrogen; the temperature of the raw material liquid is 40 ℃, the pressure is 2.2MPA (absolute pressure), the gas phase fraction is 0, the mole fraction of propane is 85%, the temperature of the raw material liquid after passing through the first heat exchanger 2 is 10 ℃, and the temperature of the raw material liquid after passing through the first regulating valve 3 is as follows: -30 ℃;
step two: enabling the raw material liquid passing through a first raw material liquid inlet 27 of the first rectifying tower 4 in the first step to enter the first rectifying tower 4 for rectification and purification, enabling a gas phase after rectification and purification to enter the second heat exchanger 6 for heat exchange and condensation through a gas phase outlet 28 at the top of the first rectifying tower 4 and a first raw material gas inlet 34 of the second heat exchanger 6, enabling the raw material gas after heat exchange and condensation to enter a gas-liquid separator 7 through a first raw material outlet 38 of the second heat exchanger 6 for gas-liquid separation, enabling a liquid phase to flow back into the first rectifying tower 4 through a liquid phase outlet 41 of the gas-liquid separator 7 and a second raw material inlet 29 of the first rectifying tower 4, enabling a gas phase to flow into the first heat exchanger 2 through a gas phase outlet 40 of the gas-liquid separator 7 and a second raw material inlet 19 of the first heat exchanger 2 for cold recovery, and enabling tail gas after cold recovery to be conveyed into a waste gas furnace 51 through a second raw material outlet 22 of the first heat exchanger 2 and an eighth regulating valve 11 for treatment; the temperature of the raw material gas at the gas phase outlet 28 at the top of the first rectifying tower 4 is as follows: -35.6 ℃ and the feed gas temperature at the first feed outlet 38 of the second heat exchanger 6 is: -37 ℃ and the tail gas temperature at the second feed outlet 22 of the first heat exchanger 2 is: 1 deg.C;
step three: raw material liquid at the tower bottom liquid phase outlet 31 of the first rectifying tower 4 in the second step enters the second rectifying tower 9 through the third regulating valve 5 and the first raw material inlet 46 of the second rectifying tower 9 for rectification, the rectified liquid phase enters the first heat exchanger 2 through the tower bottom liquid phase outlet 44 of the second rectifying tower 9 and the third raw material inlet 18 of the first heat exchanger 2 for heat exchange and then cold energy is recovered, and tail gas after cold energy recovery enters the waste gas furnace 51 through the third raw material outlet 23 of the first heat exchanger 2 and the ninth regulating valve 12; the rectified gas phase is divided into two parts after passing through a gas phase outlet 42 at the top of the second rectifying tower 9, a second raw material gas inlet 36 of the second heat exchanger 6 and a second raw material outlet 33 of the second heat exchanger 6, one part enters the second rectifying tower 9 through a fourth regulating valve 8 and a second raw material inlet 47 of the second rectifying tower 9 for reflux, and the other part enters a product storage tank 48 through a seventh regulating valve 10; the temperature of the raw material liquid entering the first raw material inlet 46 of the second rectifying tower 9 is as follows: -26 ℃, pressure: 0.18MPa (absolute pressure); the temperature of the raw material gas at the top gas phase outlet 42 of the second rectification column 9 is as follows: -36 ℃ and the product temperature at the second feed outlet 33 of the second heat exchanger 6 is: -37 ℃, pressure: 0.13MPa (absolute pressure), gas phase fraction of 0, and mole fraction of propane of 99.9994%;
step four: in the process of refrigeration cycle, a refrigerant in the refrigeration device 50 is divided into two streams, wherein one stream enters a third tee joint 43 after exchanging heat with a first mixed gas inlet 20 of the first heat exchanger 2 and precooling to 10 ℃, and then enters the third tee joint 43 after passing through a first mixed gas outlet 25 of the first heat exchanger 2, a fifth regulating valve 14 and a reboiler 45 of the second rectifying tower 9, the other stream enters the third tee joint 43 after passing through a second regulating valve 13 and a reboiler 30 of the first rectifying tower 4, then the two mixed liquids are mixed, throttled and depressurized through a sixth regulating valve 15, enter the second heat exchanger 6 through a mixed liquid inlet 37 of the second heat exchanger 6 to provide cold energy for the mixed liquids, so that the overhead gases of the first rectifying tower 4 and the second rectifying tower 9 are condensed and refluxed, and the gasified mixed gas enters the second heat exchanger 6 through a third outlet 35 of the second heat exchanger 6 and a second mixed gas inlet 26 of the first heat exchanger 2, and enters the second heat exchanger 6 through a second mixed gas outlet 21 of the first heat exchanger 2 and a second mixed gas inlet 16 of the second heat exchanger 2 after the cold energy is recovered in the second heat exchanger 6 to be used for cycle.
In the description of the present invention, it is to be understood that the terms "upper", "bottom", "middle", "top", and the like, indicate orientations or positional relationships based on those shown in the drawings, and are used only for convenience in describing the present invention and for simplicity in description, and do not indicate or imply that the referenced devices or elements must have a particular orientation, be constructed in a particular orientation, and be operated, and thus, are not to be construed as limiting the present invention. In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "disposed," "mounted," "attached," "connected," and the like are to be construed broadly and may be, for example, fixedly connected, integrally connected, or detachably connected; or communication between the interior of the two elements; they may be directly connected or indirectly connected through an intermediate, and those skilled in the art can understand the specific meaning of the above terms in the present invention according to specific situations. It should be noted that, in this document, "first", "second", etc. are used only for distinguishing one from another, and do not indicate their importance, order, etc. The above detailed description is only specific to possible embodiments of the present invention, and they are not intended to limit the scope of the present invention, and equivalent embodiments, modifications, and alterations without departing from the technical spirit of the present invention should be included in the scope of the present invention.
Claims (1)
1. A production process of a device for producing 5N-grade high-purity propane by adopting double-tower continuous rectification is characterized by comprising the following steps of: the production process comprises the following steps:
the method comprises the following steps: the raw material liquid in the raw material liquid storage tank (1) enters a first raw material liquid inlet (27) of a first rectifying tower (4) after passing through a first raw material inlet (17) of a first heat exchanger (2), a first raw material outlet (24) of the first heat exchanger (2) and a first regulating valve (3), and the raw material liquid is: 85# industrial propane, wherein the raw material liquid comprises the following components: propane, methane, ethane, carbon dioxide, n-butane, isobutane, water, ethylene, propylene, dimethyl ether, oxygen, nitrogen; the temperature of the raw material liquid is 40 ℃, the pressure is 2.2MPA (absolute pressure), the gas phase fraction is 0, the mole fraction of propane is 85%, the temperature of the raw material liquid after passing through the first heat exchanger (2) is 10 ℃, and the temperature of the raw material liquid after passing through the first regulating valve (3) is as follows: -30 ℃;
step two: enabling the raw material liquid passing through a first raw material liquid inlet (27) of a first rectifying tower (4) in the first step to enter the first rectifying tower (4) for rectification and purification, enabling a gas phase after rectification and purification to enter a second heat exchanger (6) through a gas phase outlet (28) at the top of the first rectifying tower (4) and a first raw material gas inlet (34) of a second heat exchanger (6) for heat exchange and condensation, enabling the raw material gas after heat exchange and condensation to enter a gas-liquid separator (7) through a first raw material outlet (38) of the second heat exchanger (6) for gas-liquid separation, enabling a liquid phase to flow back into the first rectifying tower (4) through a liquid phase outlet (41) of the gas-liquid separator (7) and a second raw material inlet (29) of the first rectifying tower (4), enabling a gas phase to flow into the first heat exchanger (2) through a gas phase outlet (40) of the gas-liquid separator (7) and a second raw material inlet (19) of the first heat exchanger (2) for cold recovery, and enabling tail gas after cold recovery to be conveyed into a raw material furnace through a second raw material outlet (22) of the first heat exchanger (2) and an eighth raw material regulating valve (11) for waste gas treatment; the raw material gas temperature of a gas phase outlet (28) at the top of the first rectifying tower (4) is as follows: -35.6 ℃ and the feed gas temperature at the first feed outlet (38) of the second heat exchanger (6) is: -37 ℃ and the tail gas temperature at the second feed outlet (22) of the first heat exchanger (2) is: 1 deg.C;
step three: in the second step, the raw material liquid at the tower bottom liquid phase outlet (31) of the first rectifying tower (4) enters the second rectifying tower (9) through the third regulating valve (5) and the first raw material inlet (46) of the second rectifying tower (9) for rectification, the rectified liquid phase enters the first heat exchanger (2) through the tower bottom liquid phase outlet (44) of the second rectifying tower (9) and the third raw material inlet (18) of the first heat exchanger (2) for heat exchange and then cold energy is recovered, and the tail gas after cold energy recovery enters the waste gas furnace (51) through the third raw material outlet (23) of the first heat exchanger (2) and the ninth regulating valve (12); the rectified gas phase is divided into two parts after passing through a gas phase outlet (42) at the top of the second rectifying tower (9), a second raw material gas inlet (36) of the second heat exchanger (6) and a second raw material outlet (33) of the second heat exchanger (6), one part enters the second rectifying tower (9) through a fourth regulating valve (8) and a second raw material inlet (47) of the second rectifying tower (9) for reflux, and the other part enters a product storage tank (48) through a seventh regulating valve (10); the temperature of the raw material liquid entering the first raw material inlet (46) of the second rectifying tower (9) is as follows: -26 ℃, pressure: 0.18MPa (absolute pressure); the temperature of the raw material gas at the top gas phase outlet (42) of the second rectifying tower (9) is as follows: -36 ℃, the product temperature of the second feed outlet (33) of the second heat exchanger (6) being: -37 ℃, pressure: 0.13MPa (absolute pressure), gas phase fraction of 0, and mole fraction of propane of 99.9994%;
step four: in the refrigeration cycle process, a refrigerant in a refrigeration device (50) is divided into two parts, wherein one part of the refrigerant is subjected to heat exchange with a first mixed gas inlet (20) of a first heat exchanger (2) and precooled to 10 ℃, then enters a third tee joint (43) after passing through a first mixed gas outlet (25) of the first heat exchanger (2), a fifth regulating valve (14) and a reboiler (45) of a second rectifying tower (9), the other part of the refrigerant enters the third tee joint (43) after passing through a second regulating valve (13) and a reboiler (30) of the first rectifying tower (4), then the two mixed liquids are mixed, then are subjected to pressure reduction by a sixth regulating valve (15), and then enter a second heat exchanger (6) through a mixed liquid inlet (37) of the second heat exchanger (6) to provide cold for the mixed liquids, so that the overhead gases of the first rectifying tower (4) and the second rectifying tower (9) are condensed and refluxed, the gasified mixed gas enters a second mixed gas inlet (26) of the second heat exchanger (6) through a third outlet (35) of the second heat exchanger (6) and a second mixed gas inlet (16) of the second heat exchanger (6), and the mixed gas inlet (16) of the second heat exchanger (6) to recycle cold energy;
the device for producing 5N-grade high-purity propane by double-tower continuous rectification comprises a raw material liquid storage tank (1), a product storage tank (48), a refrigerating device (50) and a waste gas furnace (51), wherein the raw material liquid storage tank (1) is connected with a first raw material inlet (17) of a first heat exchanger (2) through a pipeline, a first raw material outlet (24) of the first heat exchanger (2) is connected with a first raw material liquid inlet (27) of the first rectification tower (4) through a first regulating valve (3), a gas phase outlet (28) at the top of the first rectification tower (4) is connected with a first raw material gas inlet (34) of a second heat exchanger (6) through a pipeline, a first raw material outlet (38) of the second heat exchanger (6) is connected with a raw material inlet (39) of a gas-liquid separator (7) through a pipeline, a liquid phase outlet (41) of the gas-liquid separator (7) is connected with a second raw material inlet (29) of the first rectification tower (4) through a pipeline, a liquid phase outlet (31) of the first rectification tower (4) is connected with a second raw material inlet (9) of the second rectification tower bottom of the second rectification tower (9) through a third regulating valve (9), and a gas phase outlet (9) of the second rectification tower is connected with a second raw material liquid phase inlet (9) through a third rectification tower bottom of the second rectification tower (9), and a third rectification tower (9) through a third raw material inlet (9), and a third raw material inlet (9) of the first rectification tower (9), the second end of a first tee joint (49) is connected with a second raw material inlet (47) of a second rectifying tower (9) through a fourth regulating valve (8), the third end of the first tee joint (49) is connected with a product storage tank (48) through a seventh regulating valve (10), a tower bottom liquid phase outlet (44) of the second rectifying tower (9) is connected with a third raw material inlet (18) of a first heat exchanger (2) through a pipeline, a third raw material outlet (23) of the first heat exchanger (2) is connected with a waste gas furnace (51) through a ninth regulating valve (12), a gas phase outlet (40) of a gas-liquid separator (7) is connected with a second raw material inlet (19) of the first heat exchanger (2) through a pipeline, and a second raw material outlet (22) of the first heat exchanger (2) is connected with the waste gas furnace (51) through an eighth regulating valve (11);
an outlet of the refrigerating device (50) is connected with a second tee joint (32), a second end of the second tee joint (32) is connected with a first mixed gas inlet (20) of the first heat exchanger (2) through a pipeline, and a first mixed gas outlet (25) of the first heat exchanger (2) is connected with a first end of a third tee joint (43) through a fifth regulating valve (14) and a reboiler (45) of the second rectifying tower (9); the third end of the second tee joint (32) is connected with the second end of the third tee joint (43) through a second regulating valve (13) and a reboiler (30) of the first rectifying tower (4); the third end of the third tee joint (43) is connected with a mixed liquid inlet (37) of the second heat exchanger (6) through a sixth regulating valve (15), a third outlet (35) of the second heat exchanger (6) is connected with a second mixed gas inlet (26) of the first heat exchanger (2) through a pipeline, and a second mixed gas outlet (21) of the first heat exchanger (2) is connected with an inlet of the refrigerating device (50) through a tenth regulating valve (16).
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