CN111377451A - Desorption device and method for separating hydrogen chloride from chlorosilane - Google Patents
Desorption device and method for separating hydrogen chloride from chlorosilane Download PDFInfo
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- CN111377451A CN111377451A CN202010301339.0A CN202010301339A CN111377451A CN 111377451 A CN111377451 A CN 111377451A CN 202010301339 A CN202010301339 A CN 202010301339A CN 111377451 A CN111377451 A CN 111377451A
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Abstract
The invention provides a desorption device and a method for separating hydrogen chloride from chlorosilane. This desorption device is including desorption tower, desorption tower includes the reboiler at the bottom of the tower, the tower body, the top of the tower condenser of setting at the tower body inner chamber, the tower body has the feed inlet, it takes off the thing and liquid column bottoms gets into the tower body through the feed inlet to form gaseous state after reboiler flash distillation at the bottom of the tower to wait to take off the material, gaseous state is taken off the thing and is removed the top of the tower condenser removal, desorption device still includes the intercooler, the intercooler is circulating water cooler, the refrigerated water cooler, low temperature is waited to take off the combination of one kind or several kinds among the material heat exchanger of inhaling, along the flow direction of gaseous state desorption thing, the intercooler sets up between feed. The intercooler is used for precooling the gaseous desorption object, so that the amount of the gaseous desorption object entering the tower top condenser and the content of chlorosilane in the gaseous desorption object are greatly reduced, the demand of the tower top condenser on a low-temperature refrigerant is reduced to a great extent, and the operation cost of the desorption tower is further reduced.
Description
Technical Field
The invention relates to the technical field of desorption, in particular to a desorption device and a method for separating hydrogen chloride from chlorosilane.
Background
With the continuous decrease of the price of the polysilicon, production enterprises are forced to adopt more energy-saving production processes and devices to reduce the production cost. Some hydrogen chloride inevitably generated in the production process of polycrystalline silicon needs to be separated, and the hydrogen chloride is generally separated by using a desorption tower by adopting an absorption-desorption method. According to the production requirement, high-purity liquid hydrogen chloride or high-purity gas hydrogen chloride can be obtained.
Generally, gaseous hydrogen chloride can be obtained from the desorption tower by combining the conditions of the temperature of a refrigerant and the temperature of secondary steam, wherein the pressure at the top of the tower is generally 0.6MPaG, the temperature of a condenser at the top of the tower is generally-45 to-50 ℃, the temperature of a feed plate is generally 60 to 80 ℃, the temperature of a reboiler at the bottom of the tower is generally 110 ℃, and the gradient distribution of the material temperature in the tower is larger. If liquid hydrogen chloride is to be obtained, it is advantageous that the pressure at the top of the tower is generally higher than 0.85MPa, and the reboiler temperature at the bottom of the tower is generally higher than 130 ℃, in which case high-pressure steam is required to heat the bottom of the tower. If there is no special requirement for the purity of hydrogen chloride (hydrogen chloride contains more hydrogen when hydrogen chloride is extracted from gas state, and hydrogen chloride purity is higher when hydrogen chloride is extracted from liquid state), a low-pressure desorption scheme is generally adopted, but no matter which scheme is adopted, a tower top condenser needs to use a low-temperature refrigerant with high operation cost as a cold source, a tower bottom reboiler needs to use steam as a heat source, so that the temperature distribution change of the whole tower is large, and the material distribution difference of the whole tower is large.
The desorption tower has large temperature distribution, so that cold sources with different grades can be used, the cold source with low operation cost is used for replacing the cold source with high operation cost to achieve the purpose of reducing the operation cost of the desorption tower, and particularly for the tower with large material processing capacity, the demand of the tower top for the refrigerant becomes large, so that the refrigerant cost is high.
Disclosure of Invention
The invention mainly aims to provide a desorption device and a separation method of hydrogen chloride in chlorosilane, and the desorption device and the separation method are used for solving the problem that in the prior art, the cost of a refrigerant at the top of a tower is high during hydrogen chloride desorption.
In order to achieve the above object, according to one aspect of the present invention, there is provided a desorption device, the desorption device includes a desorption tower, the desorption tower includes a tower bottom reboiler, a tower body, and a tower top condenser disposed in an inner cavity of the tower body, the tower body has a feed inlet, a material to be desorbed is flash evaporated by the tower bottom reboiler to form a gaseous desorption product and a liquid tower bottoms, the gaseous desorption product enters the tower body through the feed inlet, the gaseous desorption product moves toward the tower top condenser, the desorption device further includes an intercooler, the intercooler is one or a combination of several of a circulating water cooler, a chilled water cooler, and a low temperature material heat exchanger to be desorbed, and the intercooler is disposed between the feed inlet and the tower top condenser along a flow direction of the gaseous desorption product.
Further, the intercooler is arranged in the inner cavity of the tower body.
Further, above-mentioned intercooler includes circulating water cooler and refrigerated water cooler, and circulating water cooler and refrigerated water cooler set up in the tower body inner chamber, and the refrigerated water cooler is located circulating water cooler's top.
Further, the inner diameter of the column body below the feed port was D1, the inner diameter of the column body above the feed port was D2, and D1 > D2.
Furthermore, the inner diameter of the tower body below the feeding port is D1, the tower body above the feeding port is formed by connecting a first tower body section with the inner diameter of D2, a second tower body section with the inner diameter of D3 and a third tower body section with the inner diameter of D4, the circulating water cooler is arranged in the inner cavity of the first tower body section, the chilled water cooler is arranged in the inner cavity of the second tower body section, the tower top condenser is arranged in the inner cavity of the third tower body section, and D1 > D2 > D3 > D4.
Further, the circulating water cooler is arranged in the upper inner cavity of the first tower body section, the chilled water cooler is arranged in the upper inner cavity of the second tower body section, and the tower top condenser is arranged in the upper inner cavity of the third tower body section.
Further, the intercooler is connected and arranged outside the tower body of the desorption tower, a first interface and a second interface are arranged between the intercooler and the desorption tower, a partition plate is arranged in an inner cavity of the tower body, and the first interface, the partition plate and the second interface are sequentially arranged away from the feed inlet.
Further, the intercooler comprises a circulating water cooler and a chilled water cooler, the circulating water cooler is arranged at the upstream of the chilled water cooler and is provided with a first interface with the desorption tower, and the chilled water cooler is arranged at the upstream of the tower top condenser and is provided with a second interface with the desorption tower.
Furthermore, the desorption device also comprises a raw material preheater and a tower bottom product conveying pipeline, wherein the raw material preheater is communicated with the feeding hole, and the tower bottom product conveying pipeline penetrates through the raw material preheater to provide at least part of heat sources for the raw material preheater.
Further, the desorption device also comprises a bottom product conveying pipeline, an overhead product heat exchanger and an overhead product conveying pipeline, wherein the top product conveying pipeline and the bottom product conveying pipeline are connected with the overhead product heat exchanger so as to realize the heat exchange between the bottom product and the overhead product.
Further, the top of the desorption column has a gas separated product outlet and a liquid separated product outlet, the top product conveying pipeline comprises a gas pipeline and a liquid pipeline, and the top product heat exchanger comprises: the first tower top heat exchanger is connected with the gas separation product outlet through a gas pipeline; and the second tower top heat exchanger is connected with the liquid separation outlet through a liquid pipeline, and a tower bottom product conveying pipeline passes through the first tower top heat exchanger and/or the second tower top heat exchanger to provide at least part of heat sources for the first tower top heat exchanger and/or the second tower top heat exchanger.
Further, the tower bottom reboiler is a thermosyphon reboiler.
According to another aspect of the present invention, there is provided a method for separating hydrogen chloride from chlorosilanes, the method comprising: carrying out flash evaporation on chlorosilane liquid containing hydrogen chloride by using a tower bottom reboiler of the desorption tower to obtain a gaseous desorption substance and a liquid tower bottom substance; and sequentially cooling the gaseous desorption object by using an intercooler and condensing a tower top condenser of the desorption tower to obtain a tower top object and a reflux object, wherein the intercooler is one or a combination of a circulating water cooler, a chilled water cooler and a low-temperature heat exchanger for the material to be desorbed.
Further, the separation method also comprises the step of preheating the chlorosilane liquid before the chlorosilane liquid enters the desorption tower, preferably, liquid tower bottoms are adopted to preheat the chlorosilane liquid, preferably, the temperature of the chlorosilane liquid entering the desorption tower is 60-70 ℃, and preferably, the temperature of the chlorosilane liquid before the chlorosilane liquid is preheated is 0-30 ℃.
Further, the above separation method further comprises heating the overhead with a liquid bottoms.
Further, the pressure at the top of the desorption tower is 0.5-1.4 MPa.
Further, above-mentioned intercooler sets up in the tower body inner chamber of desorption tower, and preferred intercooler is including the circulating water cooler and the refrigerated water cooler that set gradually, and the refrigerated water cooler is located circulating water cooler's top.
Further, above-mentioned intercooler and desorption tower are connected the setting outside the tower body of desorption tower, and the intercooler and desorption tower between have first interface and second interface, be provided with the baffle in the tower body inner chamber of desorption tower, first interface, the baffle, the reboiler setting at the bottom of the tower is kept away from in proper order to the second interface, preferred intercooler includes circulating water cooler and refrigerated water cooler, and circulating water cooler and desorption tower between have first interface, the refrigerated water cooler set up the top of the tower condenser the upper reaches and the desorption tower between have the second interface.
Further, the temperature of the gaseous desorbed substances cooled by the circulating water cooler is below 45 ℃.
Further, the temperature of the gaseous desorption object cooled by the chilled water cooler is below 15 ℃.
Furthermore, the refrigerant temperature of the overhead condenser is-70 to-50 ℃.
By applying the technical scheme of the invention, the intercooler arranged in the desorption device pre-cools the gaseous desorbed substances, so that the amount of the gaseous desorbed substances entering the tower top condenser and the content of chlorosilane in the gaseous desorbed substances are greatly reduced, the demand of the tower top condenser on low-temperature refrigerants is reduced to a great extent, 78% of the demand of the tower top low-temperature refrigerants can be saved at most through measurement and calculation, and the operation cost of the desorption tower is further reduced; adopt the desorption device of this application simultaneously and before setting up the intercooler, steam temperature and steam consumption that the reboiler at the bottom of the tower used do not take place too big change, and no matter the product of top of the tower product, still the product of bottom of the tower product all maintains higher quality.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 shows a schematic structural view of a desorption apparatus provided in accordance with embodiment 1 of the present invention; and
FIG. 2 is a schematic view showing the construction of a desorption apparatus provided in accordance with embodiment 2 of the present invention;
FIG. 3 is a schematic view showing the construction of a desorption apparatus provided in accordance with embodiment 3 of the present invention;
FIG. 4 is a schematic view showing the construction of a desorption apparatus provided in accordance with embodiment 4 of the present invention;
FIG. 5 is a schematic view showing the construction of a desorption apparatus provided in accordance with embodiment 5 of the present invention;
fig. 6 shows a schematic structural view of a desorption device provided in example 6 of the present invention.
Wherein the figures include the following reference numerals:
10. a desorption tower; 11. a tower bottom reboiler; 12. a tower body; 13. a tower top condenser; 14. a partition plate;
21. a circulating water cooler; 22. a chilled water cooler; 23. a low-temperature heat exchanger for the material to be desorbed; 30. a raw material preheater; 40. a bottoms transfer line; 51. a first overhead heat exchanger; 52. a second overhead heat exchanger; 61. a gas line; 62. a liquid line.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings.
As the analysis of the background technology of the application, the temperature of the condenser at the top of the tower, the temperature of the feeding plate and the temperature of the low reboiler of the tower have larger difference, in order to control the content of chlorosilane in desorbed hydrogen chloride at lower concentration, a large amount of low-temperature refrigerants are needed to be used for keeping the condenser at the top of the tower at lower temperature, so that the operation cost of the hydrogen chloride desorption tower is higher, and in order to solve the problem, the application provides a desorption device and a separation method of hydrogen chloride in chlorosilane.
In an exemplary embodiment of the present application, a desorption device is provided, as shown in fig. 1 to 6, the desorption device includes a desorption tower 10, the desorption tower 10 includes a tower bottom reboiler 11, a tower body 12, and an overhead condenser 13 disposed in an inner cavity of the tower body 12, the tower body 12 has a feed inlet, after a material to be desorbed is flash evaporated by the tower bottom reboiler 11 to form a gaseous desorption product and a liquid tower bottom enters the tower body 12 through the feed inlet, the gaseous desorption product moves toward the overhead condenser 13, the desorption device further includes an intercooler, the intercooler is one or a combination of several of a circulating water cooler 21, a chilled water cooler 22, and a low-temperature material to be desorbed heat exchanger 23, and the intercooler is disposed between the feed inlet and the overhead condenser 13 along a flow direction of the gaseous desorption product.
The intercooler arranged in the desorption device pre-cools the gaseous desorption object, so that the amount of the gaseous desorption object entering the tower top condenser 13 and the content of chlorosilane in the gaseous desorption object are greatly reduced, the demand of the tower top condenser 13 for low-temperature refrigerants is reduced to a great extent, 78% of the demand of the tower top low-temperature refrigerants can be saved at most through measurement and calculation, and the operation cost of the desorption tower 10 is further reduced; simultaneously, before the desorption device and the intercooler are arranged, the steam temperature and the steam consumption of the tower bottom reboiler 11 are not changed greatly, and the product of the tower top product or the tower bottom product maintains high quality.
In order to better understand the above cost description, the operation cost of the low-temperature refrigerant and the chilled water is taken as an example for the following description: the running cost of the low-temperature refrigerant is different from that of the chilled water, and the low-temperature refrigerant and the chilled water also have the heat exchange quantity of 1wkcal, 17 degrees of electricity is needed for R507 at the temperature of-55 ℃, and 3 degrees of electricity is needed for the chilled water. For example, if the desorption tower 10 originally needs a refrigerant at-55 ℃, 100wkcal of heat exchange amount is needed, and the electricity consumption is 100 × 17-1700 kwh; however, the method of the invention needs 40wkcal of refrigerant at-55 ℃ and 60wkcal of chilled water, the electricity consumption is 40 × 17+60 × 3 ═ 860, the cost is reduced by 1700-
The quantity of the intercoolers can be comprehensively considered according to factors such as the types of usable public works, 10 loads of the desorption tower, the height of the tower, the equipment cost and the like, and if a plurality of intercoolers are used, the plurality of intercoolers can be connected in series. For the installation position of the intercooler, the intercooler can be placed in the tower body 12, or the intercooler can be placed at a proper height on the building, so that the liquid can flow back to the desorption tower 10 by gravity, or the intercooler can be placed at a lower position, the liquid is sent back to the desorption tower 10 by using a pump, which form is determined according to specific conditions, the installation position of the refrigerated water cooler 22 is flexible, and the refrigerated water cooler is suitable for the reconstruction of old devices.
In order to increase the degree of equipment integration of the desorption device, the intercooler is preferably arranged in the inner cavity of the tower body 12. In one embodiment, as shown in fig. 1 and 2, the intercooler includes a circulating water cooler 21 and a chilled water cooler 22, the circulating water cooler 21 and the chilled water cooler 22 are disposed in the interior of the tower 12, and the chilled water cooler 22 is located above the circulating water cooler 21. The chilled water cooler 22 can further deeply cool the gaseous desorption object cooled by the circulating water cooler 21, so that the cold energy of each cooler can be fully utilized.
In order to further control the temperature and material distribution in the column, it is preferable that the inner diameter of the column body 12 below the feed port is D1, and the inner diameter of the column body 12 above the feed port is D2, D1 > D2.
In one embodiment, as shown in fig. 1 or 2, the inner diameter of the tower body 12 below the feed inlet is D1, the tower body 12 above the feed inlet is formed by connecting a first tower body section with an inner diameter of D2, a second tower body section with an inner diameter of D3 and a third tower body section with an inner diameter of D4, the circulating water cooler 21 is arranged in the inner cavity of the first tower body section, the chilled water cooler 22 is arranged in the inner cavity of the second tower body section, and the overhead condenser 13 is arranged in the inner cavity of the third tower body section, wherein D1 > D2 > D3 > D4. The gas-liquid separation effect of the cooled materials of the coolers is improved by the arrangement of the inner diameter of the tower body 12.
Further preferably, as shown in fig. 1 and 2, the above-mentioned circulating water cooler 21 is provided in the upper half inner chamber of the first tower section, the chilled water cooler 22 is provided in the upper half inner chamber of the second tower section, and the overhead condenser 13 is provided in the upper half inner chamber of the third tower section. So as to improve the cooling and separating effect of each cooler and condenser.
In order to improve the universality of the desorption device of the application, preferably, as shown in fig. 5 and 6, the intercooler is connected and arranged outside the tower body 12 of the desorption tower 10, a first interface and a second interface are arranged between the intercooler and the desorption tower 10, a partition plate 14 is arranged in an inner cavity of the tower body 12, and the first interface, the partition plate 14 and the second interface are sequentially arranged away from the feed inlet. When the intercooler is connected and arranged outside the tower body 12 of the desorption tower 10, the partition plate 14 is arranged in the inner cavity of the tower body 12, so that the gaseous desorption object does not move upwards in the inner cavity of the desorption tower 10 any more and enters the intercooler for heat exchange. The structure is relatively less in change and wide in applicability.
In one embodiment, as shown in fig. 5 and 6, the intercooler includes a circulating water cooler 21 and a chilled water cooler 22, the circulating water cooler 21 is disposed upstream of the chilled water cooler 22 and has a first interface with the desorption tower 10, and the chilled water cooler 22 is disposed upstream of the overhead condenser 13 and has a second interface with the desorption tower 10. The chilled water cooler 22 can further deeply cool the gaseous desorption object cooled by the circulating water cooler 21, so that the cold energy of each cooler can be fully utilized.
The temperature of the bottom product of the desorption tower 10 is high, and in order to recycle the part of heat, as shown in fig. 1 or 2, the desorption device further comprises a raw material preheater 30 and a bottom product conveying pipeline 40, wherein the raw material preheater 30 is communicated with the feeding port, and the bottom product conveying pipeline 40 penetrates through the raw material preheater 30 to provide at least part of heat source for the raw material preheater 30. The raw materials are preheated by the tower bottom product, so that the heat of the tower bottom product is recovered, and the overall energy consumption of the process is reduced.
The refrigerant of the low-temperature material heat exchanger 23 for desorption is the material to be desorbed which is not preheated, and the heat exchanger is used for exchanging heat between the material to be desorbed and the gaseous desorption object, so that the preheating of the material to be desorbed is realized, and therefore, if the low-temperature material heat exchanger 23 for desorption is used as an intercooler, the raw material preheater 30 can not be separately arranged. As shown in fig. 3 and 4.
The desorption tower 10 can further process the tower top product by controlling the tower top pressure, for example, when the hydrogen chloride in the chlorosilane liquid is desorbed, the tower top product is mainly a mixture of hydrogen chloride and hydrogen, and the liquid mixture of hydrogen chloride and hydrogen can be obtained by controlling the tower top pressure, and the liquid hydrogen chloride and gaseous hydrogen can also be obtained.
In one embodiment of the present application, as shown in fig. 1 to 6, the desorption device further comprises a bottom product transfer line 40, an overhead product heat exchanger and an overhead product transfer line, wherein the overhead product transfer line and the bottom product transfer line 40 are connected with the overhead product heat exchanger to realize the heat exchange between the bottom product and the overhead product. The tower top product is heated in the tower top product heat exchanger by utilizing the tower bottom product, so that the heat of the tower bottom product is recovered on one hand, and the temperature of the mixture of the hydrogen chloride and the hydrogen at the tower top is increased to recover or utilize the hydrogen chloride and the hydrogen on the other hand.
In another embodiment of the present application, as shown in FIG. 2, the top of the desorber 10 has a gas isolate outlet and a liquid isolate outlet, the overhead product transfer line comprises a gas line 61 and a liquid line 62, the overhead product heat exchanger further comprises a first overhead heat exchanger 51 and a second overhead heat exchanger 52, the first overhead heat exchanger 51 is connected to the gas isolate outlet by the gas line 61; the second overhead heat exchanger 52 is connected to the liquid separator outlet via a liquid line 62 and the bottoms transfer line 40 passes through the first and/or second overhead heat exchangers 51, 52 to provide at least part of the heat source for the first and/or second overhead heat exchangers 51, 52. And respectively carrying out heat exchange treatment on the gas separator and the liquid separator so as to be beneficial to respective recovery and utilization.
The bottoms reboiler 11 used in the present application may be a bottoms reboiler 11 of a structure commonly used in the art, and preferably the bottoms reboiler 11 is a thermosyphon reboiler to improve material handling efficiency.
The desorption device is used for desorption of chlorosilane. In another exemplary embodiment of the present application, there is provided a method for separating hydrogen chloride from chlorosilanes, the method comprising: carrying out flash evaporation on chlorosilane liquid containing hydrogen chloride by using a tower bottom reboiler 11 of a desorption tower 10 to obtain a gaseous desorption product and a liquid tower bottom; and cooling the gaseous desorption object by using an intercooler and condensing the gaseous desorption object by using a tower top condenser 13 in sequence to obtain a tower top object and a reflux object, wherein the intercooler is one or a combination of a plurality of circulating water cooler 21, a chilled water cooler 22 and a low-temperature material to be desorbed heat exchanger 23. The separation process is preferably carried out using the previously described desorption device.
The gaseous desorbed substances are pre-cooled by the intercooler, so that the amount of the gaseous desorbed substances entering the tower top condenser 13 and the content of chlorosilane in the gaseous desorbed substances are greatly reduced, the demand of the tower top condenser 13 on low-temperature refrigerants is reduced to a great extent, 78% of the demand of the tower top low-temperature refrigerants can be saved at most through measurement and calculation, and the operation cost of the desorption tower 10 is further reduced; meanwhile, before the desorption method and the intercooler are adopted, the steam temperature and the steam consumption of the tower bottom reboiler 11 are not obviously changed, and the product quality of the tower top product or the tower bottom product is maintained to be high.
In order to save the energy consumption for operating the desorption tower 10, it is preferable that the separation method further comprises preheating the chlorosilane liquid before entering the desorption tower 10, and preferably preheating the chlorosilane liquid with the liquid column bottom. For example, chlorosilane liquid which is lower than normal temperature and absorbs hydrogen chloride is sent into a desorption tower 10, heated to a temperature close to a bubble point by liquid tower bottoms before the chlorosilane liquid enters the desorption tower 10, and then enters the desorption tower 10 to be flashed to obtain gaseous desorption products and liquid tower bottoms. In one embodiment, the temperature of the chlorosilane liquid entering the desorption tower 10 is preferably 60-70 ℃, and the temperature of the chlorosilane liquid before preheating is preferably 0-30 ℃.
In one embodiment, to achieve heat recovery from the liquid bottoms, it is preferred that the separation process further comprises heating the overheads with the liquid bottoms. The liquid tower bottom is chlorosilane liquid without hydrogen chloride, the chlorosilane liquid is preheated and then the tower top is heated, part of the liquid tower bottom after being cooled can be sent to a hydrogen chloride absorption device, and the rest part of the liquid tower bottom can be sent to a chlorosilane rectifying tower.
Different tower tops can be obtained by controlling the tower top pressure, for example, when the tower top pressure of the desorption tower 10 is controlled to be 0.5-1.4 MPa, the obtained tower top is a mixture of hydrogen and hydrogen chloride. When the pressure at the top of the desorption column 10 is controlled to be above 0.85MPa, for example, 0.95MPa, the obtained overhead is hydrogen gas and liquid hydrogen chloride.
The quantity of the intercoolers can be comprehensively considered according to factors such as the types of usable public works, 10 loads of the desorption tower, the height of the tower, the equipment cost and the like, and if a plurality of intercoolers are used, the plurality of intercoolers can be connected in series. For the installation position of the intercooler, the intercooler can be placed in the tower body 12, or the intercooler can be placed at a proper height on the building, so that the liquid can flow back to the desorption tower 10 by gravity, or the intercooler can be placed at a lower position, the liquid is sent back to the desorption tower 10 by using a pump, which form is determined according to specific conditions, the installation position of the refrigerated water cooler 22 is flexible, and the refrigerated water cooler is suitable for the reconstruction of old devices.
In order to increase the degree of integration of the equipment, it is preferable that an intercooler is disposed in the inner cavity of the tower body 12 of the desorption tower 10. It is further preferable that the intercooler includes a circulating water cooler 21 and a chilled water cooler 22 which are arranged in this order, and the chilled water cooler 22 is located above the circulating water cooler 21. The chilled water cooler 22 can further deeply cool the gaseous desorption object cooled by the circulating water cooler 21, so that the cold energy of each cooler can be fully utilized.
In order to improve the universality of the separation method, preferably, the intercooler is connected with the desorption tower 10 and arranged outside the tower body 12 of the desorption tower 10, a first interface and a second interface are arranged between the intercooler and the desorption tower 10, a partition plate 14 is arranged in the inner cavity of the tower body 12 of the desorption tower 10, and the first interface, the partition plate 14 and the second interface are sequentially far away from the tower bottom reboiler 11. When the intercooler is connected and arranged outside the tower body 12 of the desorption tower 10, the partition plate 14 is arranged in the inner cavity of the tower body 12, so that the gaseous desorption object does not move upwards in the inner cavity of the desorption tower 10 any more and enters the intercooler for heat exchange. The structure is relatively less in change and wide in applicability. Preferably, the intercooler includes a circulating water cooler 21 and a chilled water cooler 22, and the circulating water cooler 21 has a first interface with the desorption tower 10, and the chilled water cooler 22 is disposed upstream of the overhead condenser 13 and has a second interface with the desorption tower 10. The chilled water cooler 22 can further deeply cool the gaseous desorption object cooled by the circulating water cooler 21, so that the cold energy of each cooler can be fully utilized.
In order to improve the cooling efficiency of each cooler, the supply temperature of the circulating water in the circulating water cooler 21 is preferably 30 to 35 ℃ so that the temperature of the gaseous desorbed substances cooled by the circulating water cooler 21 is 45 ℃ or lower. The supply temperature of the chilled water cooler 22 is preferably 5 to 10 ℃ so that the temperature of the gaseous desorbed substances cooled by the chilled water cooler 22 is below 15 ℃. The refrigerant temperature of the overhead condenser 13 is preferably-70 to-50 ℃.
The advantageous effects of the present application will be further described below with reference to examples and comparative examples.
Example 1
Referring to fig. 1, gaseous hydrogen chloride is extracted from the top of the desorption tower 10. The method comprises the steps of feeding chlorosilane liquid which is at a temperature of 0-30 ℃ and has absorbed hydrogen chloride and has a pressure of more than 0.65MPa into a desorption tower 10, wherein the mass content of the hydrogen chloride in the chlorosilane liquid is about 0.004, heating the chlorosilane liquid to a temperature close to a bubble point in a raw material preheater 30 before the chlorosilane liquid enters the desorption tower 10, and flashing the chlorosilane liquid after the chlorosilane liquid enters the desorption tower 10 to obtain a gaseous desorption product and a liquid tower bottom, wherein the liquid tower bottom is the chlorosilane liquid without hydrogen chloride and hydrogen, and the gaseous desorption product is a mixture of hydrogen and hydrogen chloride mixed with part of the chlorosilane liquid. The gaseous desorption object passes through a circulating water cooler 21 at normal temperature and a freezing water cooler 22 at lower temperature, and after the rising steam and the falling liquid are sequentially and simultaneously cooled to low enough temperature, the steam quantity entering the tower top condenser 13 and the content of chlorosilane in the gas phase are reduced relative to the content before the freezing water cooler 22 is arranged, the gas phase continuously rises until the tower top condenser 13 is condensed, the tower top gas is discharged from the desorption tower 10, the liquid flows back, and the refrigerant of the tower top condenser 13 is a low-temperature refrigerant.
The height of a desorption tower 10 is about 33m, a raw material feeding hole is positioned in the middle of the tower, the packing in the tower is random packing or regular packing, preferably stainless steel pall rings, a reboiler 11 at the bottom of the tower is a thermosyphon reboiler, the temperature of circulating water is 32 ℃ supply/42 return, the temperature of freezing water is 7 ℃ supply/12 return, the temperature of low-temperature refrigerant is-55 ℃, the pressure of the top of the desorption tower 10 is about 0.6MPa, a mixture of hydrogen chloride and hydrogen with the chlorosilane volume content of less than 1%, the pressure of 0.6MPa and the temperature of-45 to-50 ℃ is obtained by a condenser 13 at the top of the tower, and the gas temperature can be increased to 40-60 ℃ after passing through a hydrogen chloride heater. The temperature of the liquid tower bottom is 110-120 ℃, the temperature of the chlorosilane is reduced to 50-70 ℃ after passing through the raw material preheater 30 and the hydrogen chloride heater, one part of the chlorosilane is sent to the hydrogen chloride absorption device, and the rest chlorosilane is sent to the chlorosilane rectifying tower. The mixture of hydrogen chloride and hydrogen obtained from the overhead condenser 13 is heated by a hydrogen chloride heater and sent to a tank field or other processes.
Wherein, through calculation, if the process and the equipment of the invention are not adopted, each treatment time is 100m3-11 ten thousand kcal of chlorosilane liquid overhead refrigerant; after the process and the equipment are adopted, every 100m of treatment is carried out3-the chlorosilane liquid overhead refrigerant demand is 3.3 kilo-cal, and the chilled water demand is 16m3Therefore, the overall refrigerant demand is reduced.
Example 2
Referring to fig. 2, liquid hydrogen chloride is produced at the top of the desorption tower 10. The method comprises the steps of feeding chlorosilane liquid which is at the temperature of 10-30 ℃ and has absorbed hydrogen chloride and has the pressure of more than 0.95MPa into a desorption tower 10, wherein the mass content of the hydrogen chloride in the chlorosilane liquid is about 0.004, heating the chlorosilane liquid to the temperature of 60-70 ℃ close to a bubble point in a raw material preheater 30 before the chlorosilane liquid enters the desorption tower 10, and flashing the chlorosilane liquid after the chlorosilane liquid enters the desorption tower 10 to obtain a gaseous desorption product and a liquid tower bottom product, wherein the liquid tower bottom product is the chlorosilane liquid without hydrogen chloride and hydrogen, and the gaseous desorption product is a mixture of hydrogen and hydrogen chloride mixed with part of the chlorosilane liquid. The gaseous desorption object passes through a circulating water cooler 21 at normal temperature and a freezing water cooler 22 at lower temperature, and after the ascending steam and the falling liquid are sequentially and simultaneously cooled to low enough temperature, the steam quantity entering the overhead condenser 13 and the content of chlorosilane in the gas phase are reduced relative to the content before the freezing water cooler 22 is arranged, the gas phase continuously rises to the overhead condenser 13 to be condensed, the overhead gas is discharged from the desorption tower 10, and the liquid flows back. The refrigerant of the overhead condenser 13 is a low-temperature refrigerant.
The tower height of the desorption tower 10 is about 33m, the position of a raw material feed inlet is located in the middle of the tower, a stainless steel pall ring is used as a filler in the tower, a reboiler 11 at the bottom of the tower is a thermosyphon reboiler, the circulating water temperature is 32 ℃ supply/42 return, the freezing water temperature is 7 ℃ supply/12 return, the low-temperature refrigerant temperature is-55 ℃, the pressure at the top of the desorption tower 10 is about 0.9Mpa, a mixture of hydrogen chloride and hydrogen with the chlorosilane volume content of less than 1%, the pressure of 0.9Mpa and the temperature of-50 ℃ and liquid HCl are obtained by a condenser 13 at the top of the tower, and the liquid temperature of the liquid HCl can be increased to 40-60 ℃ after passing through a hydrogen chloride heater. The temperature of the liquid tower bottom is about 130 ℃, the temperature of the chlorosilane is reduced to 50-70 ℃ after passing through the raw material preheater 30 and the hydrogen chloride heater, one part of the chlorosilane is sent to the hydrogen chloride absorption device, and the rest chlorosilane is sent to the chlorosilane rectifying tower.
Wherein, through calculation, if the process and the equipment of the invention are not adopted, each treatment time is 100m3-chlorosilane liquid overhead refrigerant demand is 10 kcal; after the process and the equipment are adopted, every 100m of treatment is carried out3The required amount of chlorosilane liquid overhead refrigerant is 6.6 kilo-cal, and the required amount of chilled water cooler 22 is 6.7m3Therefore, the overall refrigerant demand is reduced.
It should be noted that, when the liquid hydrogen chloride is extracted from the top of the desorption tower 10, only about 10-40% of the hydrogen chloride in the raw material is extracted in a liquid form, and the rest hydrogen chloride still needs to be extracted together with the hydrogen in a gas form. If the amount of the liquid hydrogen chloride produced is increased, the pressure of the desorption tower 10 may be increased, or the temperature of the overhead condenser 13 may be continuously decreased, so that the operation cost of the desorption tower 10 may be further increased.
Example 3
Referring to fig. 3, gaseous hydrogen chloride is extracted from the top of the desorption tower 10.
Different from the embodiment 1, only the low-temperature heat exchanger 23 for the material to be desorbed is arranged in the desorption tower 10 as an intercooler, the low-temperature material is the raw material which is not preheated and has the temperature of about 3 ℃, and the raw material enters the raw material preheater 30 after passing through the low-temperature heat exchanger 23 for the material to be desorbed.
Wherein, through calculation, if the process and the equipment of the invention are not adopted, each treatment time is 100m3The required amount of chlorosilane liquid overhead refrigerant is 11 ten thousand kcal; after the process and the equipment are adopted, every 100m of treatment is carried out3The required quantity of chlorosilane liquid tower top refrigerant is 2.4 ten thousand kcal, and no freezing water or circulating water is needed, so that the whole refrigerant required quantity is reduced.
Example 4
Referring to fig. 4, liquid hydrogen chloride is produced at the top of the desorption tower 10.
Different from the embodiment 2, only the heat exchanger 23 for the low-temperature material to be desorbed is arranged in the desorption tower 10 as the intercooler, the low-temperature material is the raw material which is not preheated and has the temperature of about 3 ℃, and the raw material enters the raw material preheater 30 after being subjected to heat exchange by the intercooler.
Wherein, through calculation, if the process and the equipment of the invention are not adopted, each treatment time is 100m3The required amount of chlorosilane liquid overhead refrigerant is 10 ten thousand kcal; after the process and the equipment are adopted, every 100m of treatment is carried out3The required quantity of chlorosilane liquid tower top refrigerant is 3.3 ten thousand kcal, and chilled water and circulating water are not needed any more, so the required quantity of the whole refrigerant is reduced.
Example 5
Referring to fig. 5, gaseous hydrogen chloride is extracted from the top of the desorption tower 10.
Different from the embodiment 1, the built-in circulating water cooler 21 and the built-in chilled water cooler 22 are replaced by the built-in circulating water cooler 21 and the built-in chilled water cooler 22, and the partition plate 14 is arranged in the desorption tower 10. The energy efficiency was calculated to be substantially equivalent to that of example 1.
Example 6
Referring to fig. 6, liquid hydrogen chloride is produced at the top of the desorption tower 10.
Different from the embodiment 2, the built-in circulating water cooler 21 and the built-in chilled water cooler 22 are replaced by the external circulating water cooler 21 and the external chilled water cooler 22, and the partition plate 14 is arranged in the desorption tower 10. The energy efficiency was calculated to be substantially equivalent to that of example 2.
From the above description, it can be seen that the above-described embodiments of the present invention achieve the following technical effects:
the intercooler arranged in the desorption device pre-cools the gaseous desorption object, so that the amount of the gaseous desorption object entering the tower top condenser and the content of chlorosilane in the gaseous desorption object are greatly reduced, the demand of the tower top condenser on low-temperature refrigerants is reduced to a great extent, 78% of the demand of the tower top low-temperature refrigerants can be saved at most through measurement and calculation, and the operation cost of the desorption tower is further reduced; adopt the desorption device of this application simultaneously and before setting up the intercooler, steam temperature and steam consumption that the reboiler at the bottom of the tower used do not take place too big change, and no matter the product of top of the tower product, still the product of bottom of the tower product all maintains higher quality.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (21)
1. A desorption device comprises a desorption tower (10), the desorption tower (10) comprises a tower bottom reboiler (11), a tower body (12) and a tower top condenser (13) arranged in an inner cavity of the tower body (12), the tower body (12) is provided with a feed inlet, gaseous desorption materials and liquid tower bottom materials which are formed after the desorption materials are flashed by a tower bottom reboiler (11) enter the tower body (12) through the feed inlet, the gaseous desorption materials move to the tower top condenser (13), the device is characterized by further comprising an intercooler, wherein the intercooler is one or a combination of a plurality of circulating water cooler (21), chilled water cooler (22) and low-temperature material heat exchanger (23) to be desorbed, and is arranged between the feed inlet and the tower top condenser (13) along the flowing direction of the gaseous desorption material.
2. The desorption device according to claim 1, wherein the intercooler is arranged in the inner cavity of the tower body (12).
3. The desorption device according to claim 2, wherein the intercooler comprises the circulating water cooler (21) and the chilled water cooler (22), the circulating water cooler (21) and the chilled water cooler (22) are arranged in the inner cavity of the tower body (12), and the chilled water cooler (22) is positioned above the circulating water cooler (21).
4. The desorption apparatus according to claim 1, wherein the internal diameter of the tower body (12) below the feed inlet is D1, and the internal diameter of the tower body (12) above the feed inlet is D2, D1 > D2.
5. The desorption device according to claim 3, wherein the inner diameter of the tower body (12) below the feed inlet is D1, the tower body (12) above the feed inlet is formed by connecting a first tower body section with the inner diameter of D2, a second tower body section with the inner diameter of D3 and a third tower body section with the inner diameter of D4, the circulating water cooler (21) is arranged in the inner cavity of the first tower body section, the chilled water cooler (22) is arranged in the inner cavity of the second tower body section, and the overhead condenser (13) is arranged in the inner cavity of the third tower body section, wherein D1 > D2 > D3 > D4.
6. The desorption apparatus as set forth in claim 5 wherein the circulating water cooler (21) is disposed in the upper interior chamber of the first tower section, the chilled water cooler (22) is disposed in the upper interior chamber of the second tower section, and the overhead condenser (13) is disposed in the upper interior chamber of the third tower section.
7. The desorption device according to claim 1, wherein the intercooler is connected and arranged outside a tower body (12) of the desorption tower (10), a first port and a second port are arranged between the intercooler and the desorption tower (10), a partition plate (14) is arranged in an inner cavity of the tower body (12), and the first port, the partition plate (14) and the second port are sequentially arranged away from the feed inlet.
8. The desorption apparatus according to claim 7, characterized in that the intercooler comprises the circulating water cooler (21) and the chilled water cooler (22), the circulating water cooler (21) being arranged upstream of the chilled water cooler (22) with the first interface to the desorption column (10), the chilled water cooler (22) being arranged upstream of the overhead condenser (13) with the second interface to the desorption column (10).
9. The desorption apparatus according to claim 1, further comprising a feed preheater (30) and a bottoms transfer line (40), the feed preheater (30) being in communication with the feed inlet, the bottoms transfer line (40) providing at least a portion of a heat source for the feed preheater (30) through the feed preheater (30).
10. The desorber device as claimed in claim 1 further comprising a bottoms transfer line (40), an overhead heat exchanger and an overhead transfer line, the overhead transfer line and the bottoms transfer line (40) being connected to the overhead heat exchanger to effect heat exchange of bottoms with overheads.
11. The desorber device as claimed in claim 10 wherein the top of the desorber (10) has a gas separator outlet and a liquid separator outlet, the top product transfer line comprises a gas line (61) and a liquid line (62), and the top product heat exchanger (50) comprises:
a first overhead heat exchanger (51) connected to said gas separation outlet via said gas line (61);
a second overhead heat exchanger (52) connected to the liquid separator outlet via the liquid line (62), the bottoms transfer line (40) passing through the first (51) and/or second (52) overhead heat exchangers to provide at least part of the heat source to the first (51) and/or second (52) overhead heat exchangers.
12. The desorption apparatus according to claim 1 wherein the bottom reboiler (11) is a thermosiphon reboiler.
13. A method for separating hydrogen chloride from chlorosilane is characterized by comprising the following steps:
carrying out flash evaporation on chlorosilane liquid containing hydrogen chloride by using a tower bottom reboiler (11) of a desorption tower (10) to obtain a gaseous desorption substance and a liquid tower bottom;
and sequentially cooling the gaseous desorption object by using an intercooler and condensing the overhead condenser (13) of the desorption tower (10) to obtain the overhead object and the reflux object, wherein the intercooler is one or a combination of a circulating water cooler (21), a chilled water cooler (22) and a low-temperature heat exchanger (23) for the material to be desorbed.
14. The separation method according to claim 13, further comprising preheating the chlorosilane liquid before entering the desorption tower (10), preferably preheating the chlorosilane liquid by using the liquid column bottoms, preferably wherein the temperature of the chlorosilane liquid entering the desorption tower (10) is 60-70 ℃, preferably the temperature of the chlorosilane liquid before preheating is 0-30 ℃.
15. The separation process of claim 13, further comprising heating the overhead with liquid bottoms.
16. The separation method according to claim 13, wherein the pressure at the top of the desorption column (10) is 0.5 to 1.4 MPa.
17. The separation method according to claim 13, wherein the intercooler is arranged in the inner cavity of the tower body (12) of the desorption tower (10), preferably the intercooler comprises a circulating water cooler (21) and a chilled water cooler (22) which are arranged in sequence, and the chilled water cooler (22) is positioned above the circulating water cooler (21).
18. The separation method according to claim 13, characterized in that the intercooler is connected with the desorption tower (10) and is arranged outside the tower body (12) of the desorption tower (10), and a first interface and a second interface are arranged between the intercooler and the desorption tower (10), a clapboard (14) is arranged in the inner cavity of the tower body (12) of the desorption tower (10), the first interface, the clapboard (14) and the second interface are sequentially arranged away from the tower bottom reboiler (11), preferably the intercooler comprises the circulating water cooler (21) and the chilled water cooler (22), and the first interface is arranged between the circulating water cooler (21) and the desorption tower (10), the chilled water cooler (22) is disposed upstream of the overhead condenser (13) and has the second interface with the desorber (10).
19. The separation method according to claim 17, wherein the temperature of the gaseous desorbent after cooling by the circulating water cooler (21) is below 45 ℃.
20. The separation method according to claim 17, characterized in that the temperature of the gaseous desorbent after cooling by the chilled water cooler (22) is the chilled water cooler (22) below 15 ℃.
21. The separation method according to claim 13, wherein the refrigerant temperature of the overhead condenser (13) is-70 to-50 ℃.
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| CN202010301339.0A CN111377451A (en) | 2020-04-16 | 2020-04-16 | Desorption device and method for separating hydrogen chloride from chlorosilane |
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| CN202010301339.0A CN111377451A (en) | 2020-04-16 | 2020-04-16 | Desorption device and method for separating hydrogen chloride from chlorosilane |
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