CN102009979B - Method for performing rectification and purification on trichlorosilane by using circulating heat - Google Patents
Method for performing rectification and purification on trichlorosilane by using circulating heat Download PDFInfo
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- CN102009979B CN102009979B CN2010106019253A CN201010601925A CN102009979B CN 102009979 B CN102009979 B CN 102009979B CN 2010106019253 A CN2010106019253 A CN 2010106019253A CN 201010601925 A CN201010601925 A CN 201010601925A CN 102009979 B CN102009979 B CN 102009979B
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Abstract
The invention relates to a method for performing rectification and purification on trichlorosilane by using circulating heat. A cyclic liquid flow passage is formed among a trichlorosilane synthetic furnace, a rectification column and a hydrogen chloride synthetic furnace; the liquid flow passage comprises a clod flow slot, a trichlorosilane synthetic furnace clamping sleeve, a hydrogen chloride synthetic furnace clamping sleeve, and clamp sleeves on a hot flow slot and the rectification column which are connected in turn; the trichlorosilane synthetic furnace clamping sleeve and the hydrogen chloride synthetic furnace clamping sleeve are connected in parallel between the clod flow slot and the hot flow slot; and heat in the hydrogen chloride synthetic furnace and the trichlorosilane synthetic furnace is used for rectification and purification of trichlorosilane in the rectification column through the control of a control system and a heat-transfer medium in the liquid flow passage, so that the recycling of heat in the system is realized. Moreover, a heat-transfer medium flowing out of the hot flow slot can be used for the preheating of nitrogen, so that the recycling of heat is realized and production cost is saved.
Description
Technical field
What the present invention relates to is a kind of method of trichlorosilane rectification and purification, particularly a kind of method of utilizing cycling hot trichlorosilane to be carried out rectification and purification.
Background technology
At present, trichlorosilane production (comprising hydrogenation of silicon tetrachloride production trichlorosilane) chemical reaction is as follows: Si+3HCl=SiHCl3+H2; Si+4HCl=SiCl4+2H2; Hydrogenation 3SiCl4+2H2+Si=4SiCl3.Main device synthetic furnace, its refrigerating unit are the internal and external casing structure.A kind of method of cooling is: the interior pipe of hot water from sleeve pipe enters the bottom (jacket exterior is the exothermic heat of reaction district) of pipe, and heat is taken away in vaporization in the bottom, discharges from the gap between the interior pipe outer tube; The another kind of type of cooling is: the low temperature thermal oil enters the bottom from interior pipe and is heated, and high temperature oil is discharged from the inner and outer pipes gap, cools off, circulated, also heat conduction cooling of hull outside.Owing to be by interior pipe direct heat transfer all, there are the common shortcoming in this two kinds of methods and device: 1. owing to wearing and tearing, corrosion and reaction produce the hydrogen embrittlement that hydrogen causes, impact pipe, be easy to damage interior pipe; Pipe is in case damage makes water (or thermal oil) enter material system, and water and SiHCl3, SiCl4 vigorous reaction cause obstruction, the damage of back processing apparatus, even blast, and thermal oil enters material, is difficult to cleaning and separates.2. owing to this kind limitation of design, cause the inequality of arranging of cooling tube, the amount inequality of water inlet (or oil) causes temperature deviation big at reaction zone, reacts undesirable.And be not used after the transfer of heat, do not meet the design concept of energy-saving and emission-reduction on the engineering science, therefore, providing a kind of can be significant the heat cyclic utilization method that produces in the trichlorosilane synthetic system.
China's application 200710018582.6, CN101125654A discloses a kind of large-scale fluidized bed reactor that trichlorosilane is produced that is used for, and comprises the conversion zone and the upper extension section of bottom; The bottom of conversion zone is provided with the silica flour opening for feed; Reactor lower part has the maintenance end socket; The maintenance end socket is provided with hydrogenchloride inlet mouth and slag-drip opening; Syngas outlet is arranged on the expanding reach; Be provided with the hydrogen chloride gas sparger between maintenance end socket and the conversion zone; Be provided with the thermal oil dactylethrae in conversion zone and the expanding reach, this thermal oil dactylethrae extends to the conversion zone bottom from expanding reach always; The top of expanding reach is provided with dactylethrae maintenance flange, and dactylethrae thermal oil inlet is arranged on the flange, and expanding reach is provided with the outlet of dactylethrae thermal oil; The outside of conversion zone is provided with the reactor half-pipe jacket, the provided with disks at two ends pipe heat conductive oil inlet of reactor half-pipe jacket and the outlet of coil pipe thermal oil.Adopt heat-conducting oil heating in the temperature rise period, adopt thermal oil shifting out reaction heat in reaction process.Temperature in the reactor enters thermal oil by temperature regulation and refers to that the low temperature oil mass of type pipe and reactor half-pipe jacket controls that it is constant.Though this device is temperature of reaction in the controlling reactor preferably, the heat that shifts out from reactor is not used, and has wasted energy consumption, has increased the weight of production cost.
In view of this, special proposition the present invention.
Summary of the invention
What the present invention relates to is that a kind of cycling hot of utilizing is carried out the method for rectification and purification to trichlorosilane, is to realize goal of the invention, and the present invention adopts following technical scheme:
A kind of method of utilizing cycling hot trichlorosilane to be carried out rectification and purification, at trichlorosilane synthetic furnace, rectifying tower, the round-robin flow passage is set between the hydrogen chloride synthetic furnace, described flow passage comprises the cold flow groove that connects successively, the trichlorosilane synthetic furnace chuck, the hydrogen chloride synthetic furnace chuck, heated launder, chuck on the rectifying tower, wherein trichlorosilane synthetic furnace chuck and hydrogen chloride synthetic furnace chuck are connected in parallel between cold flow groove and the heated launder, control by Controlling System, the rectification and purification of utilizing the heat-transfer medium in the flow passage that the heat in hydrogen chloride synthetic furnace and the trichlorosilane synthetic furnace is diverted from one use to another trichlorosilane in rectifying tower realizes the recycle of system thermal.
Described heated launder top also is provided with overflow spout, described overflow spout connects a gas-liquid heat exchanger, described gas-liquid heat exchanger is used for the preheating of nitrogen with the heat of heat-transfer medium in the overflow spout, and nitrogen enters the nitrogen heating unit after by described liquid suction heat exchanger preheating.
Described heated launder is provided with temperature sensor and fluid infusion pipeline, when the liquid temperature is higher than 80-85 ℃ in temperature sensor detects heated launder, add cold heat-transfer medium regulator solution temperature in system's control fluid infusion pipeline thermotropism chute, make it can be with preset temp 80-85 ℃ of rectifying that is used for rectifying Tata still, when liquid level reaches maximum, heat-transfer medium is discharged from overflow spout.
Described trichlorosilane synthetic furnace and hydrogen chloride synthetic furnace are provided with temperature sensor, the cold flow groove is provided with variable valve, system is by the aperture of control cold flow groove adjusted valve, and the Control Circulation flow quantity is realized the accurate control to temperature in trichlorosilane synthetic furnace and the hydrogen chloride synthetic furnace.
The heat-transfer medium of discharging from gas-liquid heat exchanger enters the device for storing liquid that links to each other with the fluid infusion pipeline and is used to regulate liquid temperature in the heated launder.
Described liquid suction heat exchanger be spiral pipe heat exchanger, spiral pipe platelet heat exchangers or in the sheet interchanger of spreading the wings.
Described nitrogen heating unit is the nitrogen electric heater, and the nitrogen after preheating enters nitrogen electric heater post-heating and is used for dry silica flour to 140-160 ℃.
Described heat-transfer medium is water or oil.
Described heated launder is divided into two Room, and wherein the water-in of chamber 1 connects the hydrogen chloride synthetic furnace chuck, and water outlet is connected with gas-liquid heat exchanger by overflow spout; The water-in of chamber 2 connects the trichlorosilane synthetic furnace chuck, and water outlet connects the rectifying tower chuck, and device for storing liquid is connected with chamber 2 by the fluid infusion pipeline in addition.
Described chamber 1 is 1 with the volume ratio of chamber 2: 2-2: 1, preferred 2: 3-4: 3, and more preferably 5: 7.
Described Controlling System is the DCS Controlling System.
Describe in detail below in conjunction with 1 pair of method of the present invention of accompanying drawing.
In trichlorosilane synthetic furnace, controlled temperature is 330-350 ℃, and silica flour and hydrogenchloride react, and produces trichlorosilane and silicon tetrachloride.Too high or too low for temperature all is disadvantageous to reaction; Temperature is too high, and silicon tetrachloride as by-product is many; Temperature is crossed low easy blowing out.Therefore, the temperature of control trichlorosilane synthetic furnace has great effect to whole synthesis technique.In addition, the synthesis temperature of hydrogenchloride, needs in time the transfer of heat in the hydrogen chloride synthetic furnace in order to keep hydrogen chloride synthetic furnace constant temperature of reaction equally up to 500 ℃.And need in the purification process of trichlorosilane rectifying tower is carried out heat treated, therefore, the contriver improves integrated artistic equipment, and the transfer of heat that trichlorosilane synthetic furnace and hydrogen chloride synthetic furnace are produced utilizes cycling hot that trichlorosilane is carried out rectification and purification to rectifying tower.
The present invention adopts water or oil to be heat-transfer medium, on trichlorosilane synthetic furnace, hydrogen chloride synthetic furnace, rectifying tower, chuck is set, after the reaction beginning, the heat-transfer medium shift reaction heat by in trichlorosilane synthetic furnace, the hydrogen chloride synthetic furnace chuck is used for the rectifying of trichlorosilane.Concrete measure is (referring to accompanying drawing 1, wherein the direction of arrow is the flow direction of heat-transfer medium in flow passage): at trichlorosilane synthetic furnace, rectifying tower, the round-robin flow passage is set between the hydrogen chloride synthetic furnace, described flow passage comprises the cold flow groove that connects successively, chuck on the trichlorosilane synthetic furnace, chuck on the hydrogen chloride synthetic furnace, heated launder, chuck on the rectifying tower, wherein chuck on the trichlorosilane synthetic furnace and the chuck on the hydrogen chloride synthetic furnace are connected in parallel between cold flow groove and the heated launder, control by Controlling System, utilize the heat-transfer medium in the flow passage that the heat in hydrogen chloride synthetic furnace and the trichlorosilane synthetic furnace is used for rectifying tower, realize the recycle of system thermal.Be equipped with temperature sensor on trichlorosilane synthetic furnace and the hydrogen chloride synthetic furnace, system is according to the aperture of the control of the temperature in synthetic furnace cold flow groove adjusted valve, the circulating fluid flow rate of trichlorosilane synthetic furnace and hydrogen chloride synthetic furnace is led in control respectively, the heat-transfer medium part that the cold flow groove is discharged enters the chuck of trichlorosilane synthetic furnace the heat in the trichlorosilane synthetic furnace is taken away, and flows to heated launder; Another part enters the chuck of hydrogen chloride synthetic furnace, behind the absorption heat, flows to heated launder equally.Be provided with temperature sensor, fluid infusion pipeline and overflow spout in the heated launder, when the heat-transfer medium temperature is higher than 80-85 ℃ in temperature sensor detects heated launder, add cold heat-transfer medium attemperation in system's control fluid infusion pipeline thermotropism chute, make the liquid stream can be with constant temp 80-85 ℃ of rectifying that is used for rectifying Tata still, the temperature that the present invention sets heat-transfer medium in the heated launder be 80-85 ℃.Because the effusive liquid temperature of trichlorosilane synthetic furnace and hydrogen chloride synthetic furnace chuck is high, therefore, must adds cold heat-transfer medium by the feeder current passage when flowing into heated launder temperature is turned down to 80-85 ℃.When liquid level reaches maximum, heat-transfer medium is discharged from overflow spout.Simultaneously be provided with variable valve on the cold flow groove, system is by the aperture of control cold flow groove adjusted valve, and the Control Circulation flow quantity is realized temperature controlling in the trichlorosilane synthetic furnace, with temperature-stable at 330-350 ℃.Controlling System of the present invention is the DCS Controlling System.Adopt technique scheme, can realize that the utilization ratio of system's heat energy reaches 75-80%.
In order further to improve the heat circulation in the trichlorosilane synthesis technique, the hot-fluid that the present invention discharges in can also overflow spout is used for the preheating (referring to accompanying drawing 2) of nitrogen.Heat-transfer medium after simultaneously heat being shifted out is used for heat recovery system once more, and concrete technical scheme is as follows:
Temperature sensor all is set on trichlorosilane synthetic furnace and hydrogen chloride synthetic furnace, Controlling System is according to the aperture of the control of the temperature in synthetic furnace cold flow groove adjusted valve, the circular flow of trichlorosilane synthetic furnace and hydrogen chloride synthetic furnace is led in control respectively, a heat-transfer medium part of discharging from the cold flow groove enters the chuck of trichlorosilane synthetic furnace the heat the trichlorosilane synthetic furnace is taken away, and flows to heated launder; Another part enters the chuck of hydrogen chloride synthetic furnace, after absorbing heat, flow to heated launder equally, temperature sensor on the heated launder detects the liquid temperature in the groove, when temperature is higher than preset range, system opens the fluid infusion pipeline thermotropism chute cold heat-transfer medium of annotating and adjusts the temperature to preset value, the present invention sets the interior liquid temperature of heated launder and is 80-85 ℃, enter rectifying Tata stills at different levels from the effusive heat-transfer medium of heated launder and keep the stable of rectifying Tata still temperature in the mode of chuck heating, control rectifying, heat shift out back the circulation again from the effusive heat-transfer medium of rectifying Tata stills at different levels and enter the chuck of trichlorosilane synthetic furnace and hydrogen chloride synthetic furnace.When the liquid level of heated launder reaches maximum, heat-transfer medium is discharged from overflow spout.Overflow spout links to each other with a gas-liquid heat exchanger, and this gas-liquid heat exchanger is used for the preheating of nitrogen with the heat of heat-transfer medium in the overflow spout, and nitrogen enters the nitrogen heating unit after by described liquid suction heat exchanger preheating.In addition, the heat-transfer medium of discharging from the solution-air interchanger can be selected to drain into the device for storing liquid that links to each other with the fluid infusion pipeline and is used to regulate liquid temperature (seeing accompanying drawing 2) in the heated launder.
Gas liquid exchanger can be for realizing any heat exchanger of gas-liquid exchange among the present invention in the prior art, the spiral pipe heat exchanger that preferred heat exchanger effectiveness is high, spiral pipe platelet heat exchangers or in the sheet interchanger of spreading the wings, when gas-liquid heat exchanger is reverse heat exchanger of spiral pipe or spiral pipe platelet heat exchangers, pneumatic outlet, liquid inlet are separately positioned on the spiral initial section of gas passage, fluid passage, and gas inlet, liquid exit then are separately positioned on the spiral rear of gas passage, fluid passage.During work, gas, liquid are along hand of spiral countercurrent flow.Thereby realize the maximization of heat recycling.The higher heat-transfer medium of temperature is discharged from coil pipe spiral tail end inflow heat exchanger and from the outlet of spiral initial section, and nitrogen enters after the venting port of coil pipe rear is discharged from the spiral initial section.Nitrogen and hot water carry out sufficient heat exchange in heat exchanger, finish the preheating of nitrogen.In addition, gas-liquid heat exchanger of the present invention can also be application number 200620034613.8 disclosed any spiral plate type gas-liquid heat exchangers or application number 01109321.8 disclosed any gas-liquid heat exchanger etc., when using other gas liquid exchanger, only need allow nitrogen and heat-transfer medium fully carry out heat exchange and get final product.Different gas liquid exchanger heat-transfer effects is variant, therefore, the utilization ratio of system of the present invention heat energy is also had certain influence, and the heat exchanger that it is good that those skilled in the art can select heat-transfer effect is realized the present invention and obtained the high utilization rate of heat.
The nitrogen of getting rid of from gas-liquid heat exchanger enters the nitrogen heating unit, and described nitrogen heating unit also can adopt any heating installation that nitrogen can be heated to 140-160 ℃ in the prior art.Preferred nitrogen electric heater of the present invention, nitrogen after preheating enters nitrogen electric heater post-heating to 140-160 ℃, utilize the raw silicon of the dry trichlorosilane of high temperature nitrogen in synthetic again, realize the recycle of heat no-discharging type in the synthetic and purification system of trichlorosilane thus.Adopt technique scheme, when adopting water as heat-transfer medium, can realize that the utilization ratio of system's heat energy reaches 80-90%, the overflow water yield reduces 70-85%, and reduce water consumption reaches 80-85%.When adopting oil as cooling media, the utilization ratio of system's heat energy reaches 85-95%.
As another kind of preferred version of the present invention, as shown in Figure 3, heated launder can also be divided into two Room, wherein the water-in of chamber 1 connects the hydrogen chloride synthetic furnace chuck, and water outlet is connected with gas-liquid heat exchanger by overflow spout; The water-in of chamber 2 connects the trichlorosilane synthetic furnace chuck, and water outlet connects the rectifying tower chuck, and device for storing liquid is connected with chamber 2 by the fluid infusion pipeline in addition.Because the heat height that the hydrogen chloride synthetic furnace chuck shifts out, in order to make full use of heat resource, to directly enter the preheating that gas-liquid heat exchanger is used for nitrogen from the effusive heat-transfer medium of hydrogen chloride synthetic furnace chuck, thereby avoided its temperature-fall period of cold medium in the fluid infusion pipeline earlier, make heat at utmost divert from one use to another preheating, improve the utilization ratio of heat in nitrogen.Can finish adjusting through fluid infusion pipeline inlet chamber 2 again to the heat-transfer medium that nitrogen carries out after the preheating to liquid temperature in the chamber 2.The present invention is by the improvement to heated launder, and the utilization ratio of system's heat energy can further improve 4-8%.The contriver has also done a large amount of experiments to the chamber 1 and the volume ratio of chamber 2 in addition, those skilled in the art know, the volume ratio of chamber 1 and chamber 2 directly has influence on the utilization of heat energy, excessive or the too small temperature of rectifying tower or synthetic furnace that all causes of ratio can not get accurate control, though also can realize the recovery of heat, can't realize the automatization control of system temperature.Therefore, the contriver determines that finally the volume ratio when chamber 1 and chamber 2 is 1: 2-2: in the time of 1, the utilization ratio of heat energy can further improve 4-8%, further reduce water consumption 5-8%, preferred 2: 3-4: 3, more preferably 5: 7, when volume ratio was 5: 7, the utilization ratio of heat energy and reduce water consumption can reach maximization.
Adopt technique scheme, the present invention has following beneficial effect:
1, adopts the DCS Controlling System that intrasystem temperature is carried out full-automation control, guaranteed the stable of temperature and the continuity of producing.
2, made full use of the heat that trichlorosilane synthetic furnace and hydrogen chloride synthetic furnace produce, realized the recycle of heat, reduced energy consumption, saved production cost, realized the utilization ratio of heat up to 80-95%.
3, the present invention is simple in structure, and economic benefit is obvious, helps applying.
Description of drawings
Fig. 1 process flow sheet of the present invention
Fig. 2 process flow sheet of the present invention
Fig. 3 process flow sheet of the present invention
Embodiment
Embodiment 1
As shown in Figure 1, the present invention is at trichlorosilane synthetic furnace, rectifying tower, the round-robin flow passage is set between the hydrogen chloride synthetic furnace, this flow passage comprises the cold flow groove that connects successively, chuck on the trichlorosilane synthetic furnace, chuck on the hydrogen chloride synthetic furnace, heated launder, chuck on the rectifying tower, wherein chuck on the trichlorosilane synthetic furnace and the chuck on the hydrogen chloride synthetic furnace are connected in parallel between cold flow groove and the heated launder, control by the DCS Controlling System, utilize the water in the flow passage that the heat in hydrogen chloride synthetic furnace and the trichlorosilane synthetic furnace is used for rectifying tower, realize the recycle of system thermal.
The present invention adopts following technical scheme to realize the recycle of heat: on trichlorosilane synthetic furnace and hydrogen chloride synthetic furnace temperature sensor is set, system is according to the aperture of the control of the temperature in each synthetic furnace cold flow groove adjusted valve, the circulating water flow of trichlorosilane synthetic furnace and hydrogen chloride synthetic furnace is led in control respectively, the water part that the cold flow groove is discharged enters the chuck of trichlorosilane synthetic furnace the heat in the trichlorosilane synthetic furnace is taken away, and flows to heated launder; Another part enters the chuck of hydrogen chloride synthetic furnace, behind the absorption heat, flows to heated launder equally.Be provided with temperature sensor, fluid infusion pipeline and overflow spout in the heated launder, when water temperature is higher than 80-85 ℃ in temperature sensor detects heated launder, add the cold water attemperation in the system control fluid infusion pipeline thermotropism chute, make the current can be with constant temp 80-85 ℃ of rectifying that is used for rectifying Tata still.The feeder current passage can be added cold water to heated launder and make that water temperature remains on 80-85 ℃ in the heated launder.When water level reaches maximum, water is discharged from overflow spout.Simultaneously be provided with variable valve on the cold flow groove, system is by the aperture of control cold flow groove adjusted valve, and Control Circulation discharge realizes the accurate control to temperature in the trichlorosilane synthetic furnace, with temperature-stable in the synthetic furnace at 330-350 ℃.Adopt technique scheme, can realize that the utilization ratio of system's heat energy reaches 75-80%.
Embodiment 2
Compare with embodiment 1, distinctive points is: overflow spout links to each other with a gas-liquid heat exchanger, and this gas-liquid heat exchanger is used for the preheating of nitrogen with the heat of water in the overflow spout, and nitrogen enters the nitrogen heating unit after by described gas-liquid heat exchanger preheating.This gas-liquid heat exchanger is the spiral pipe plate-type heat exchanger.Water after the gas-liquid heat exchange is discharged from the spiral pipe plate-type heat exchanger.Adopt this method, can realize that the utilization ratio of system thermal reaches 80-85%, reduce water consumption reaches 70-75%.
Embodiment 3
Compare with embodiment 2, distinctive points only is: the water after the gas-liquid heat exchange drains into the device for storing liquid that links to each other with the fluid infusion pipeline and is used to regulate liquid temperature in the heated launder.(see figure 2) adopts this method, can realize that the utilization ratio of system thermal reaches 80-90%, and the overflow water yield reduces 70-85%, and reduce water consumption reaches 80-85%.
Embodiment 4
Compare with embodiment 1, distinctive points only is: heat-transfer medium is oil, and the utilization ratio of system thermal reaches 75-85%.
Embodiment 5
Compare with embodiment 3, distinctive points only is: heat-transfer medium is oil, and the utilization ratio of system thermal reaches 85-95%.
Embodiment 6
Compare with embodiment 2, distinctive points only is: gas-liquid heat exchanger is application number 200620034613.8 disclosed spiral plate type gas-liquid heat exchangers, and the utilization ratio of system thermal reaches 85-90%.
Embodiment 6
Compare with embodiment 5, distinctive points only is: gas-liquid heat exchanger is application number 01109321.8 a disclosed gas-liquid heat exchanger, and the utilization ratio of system thermal reaches 90-95%.
Embodiment 7
Compare with embodiment 6, distinctive points only is: the gas-liquid heat exchanger sheet interchanger of spreading the wings in being.
Embodiment 8
As shown in Figure 3, compare with embodiment 1, distinctive points only is: hot water tank is divided into two Room, chamber 1 is 1 with the volume ratio of chamber 2: 2-2: 1 o'clock, the utilization ratio of heat energy can further improve 4-8%, further reduce water consumption 5-8%, preferred 2: 3-4: 3, more preferably 5: 7, when volume ratio was 5: 7, the utilization ratio of heat energy and reduce water consumption can reach maximization.
Embodiment 8
As shown in Figure 3, compare with embodiment 3,4, distinctive points only is: hot water tank is divided into two Room, and it is 1: 2,2: 3 that the volume ratio of chamber 1 and chamber 2 is respectively.
Embodiment 9
As shown in Figure 3, compare with embodiment 5,6, distinctive points only is: hot water tank is divided into two Room, and chamber 1 is 4: 3,2: 1 with the volume ratio of chamber 2.
Embodiment 10
As shown in Figure 3, compare with embodiment 6, distinctive points only is: hot water tank is divided into two Room, and chamber 1 is 5: 7 with the volume ratio of chamber 2.
The foregoing description only is that the preferred embodiments of the present invention are described; be not that design of the present invention and scope are limited; under the prerequisite that does not break away from design philosophy of the present invention; the professional and technical personnel makes technical scheme of the present invention in this area various variations, combination and improvement all belong to protection scope of the present invention.
Claims (9)
1. method of utilizing cycling hot trichlorosilane to be carried out rectification and purification, it is characterized in that: at trichlorosilane synthetic furnace, rectifying tower, the round-robin flow passage is set between the hydrogen chloride synthetic furnace, described flow passage comprises the cold flow groove that connects successively, the trichlorosilane synthetic furnace chuck, the hydrogen chloride synthetic furnace chuck, heated launder, chuck on the rectifying tower, wherein trichlorosilane synthetic furnace chuck and hydrogen chloride synthetic furnace chuck are connected in parallel between cold flow groove and the heated launder, control by Controlling System, the rectification and purification of utilizing the heat-transfer medium in the flow passage that the heat in hydrogen chloride synthetic furnace and the trichlorosilane synthetic furnace is diverted from one use to another trichlorosilane in rectifying tower realizes the recycle of system thermal; Described heated launder top also is provided with overflow spout, described overflow spout connects a gas-liquid heat exchanger, described gas-liquid heat exchanger is used for the preheating of nitrogen with the heat of heat-transfer medium in the overflow spout, and nitrogen enters the nitrogen heating unit after by described gas-liquid heat exchanger preheating; Described heated launder is provided with temperature sensor and fluid infusion pipeline, when the liquid temperature surpasses preset temp in temperature sensor detects heated launder, add cold heat-transfer medium regulator solution temperature in system's control fluid infusion pipeline thermotropism chute, make it can be used for the rectifying of rectifying Tata still with 80-85 ℃ preset temp, when liquid level reaches maximum, heat-transfer medium is discharged from overflow spout; Described trichlorosilane synthetic furnace and hydrogen chloride synthetic furnace are provided with temperature sensor, the cold flow groove is provided with variable valve, system is by the aperture of control cold flow groove adjusted valve, and the Control Circulation flow quantity is realized the accurate control to temperature in trichlorosilane synthetic furnace and the hydrogen chloride synthetic furnace.
2. method according to claim 1 is characterized in that: the heat-transfer medium of discharging from gas-liquid heat exchanger enters the device for storing liquid that links to each other with the fluid infusion pipeline and is used to regulate liquid temperature in the heated launder.
3. method according to claim 1 is characterized in that: described gas-liquid heat exchanger be spiral pipe heat exchanger, spiral pipe platelet heat exchangers or in the sheet interchanger of spreading the wings.
4. method according to claim 1 is characterized in that: described nitrogen heating unit is the nitrogen electric heater, and the nitrogen after preheating enters nitrogen electric heater post-heating and is used for dry silica flour to 140-160 ℃.
5. according to each described method of claim 1-4, it is characterized in that: described heat-transfer medium is water or oil.
6. according to each described method of claim 1-4, it is characterized in that: described heated launder is divided into two Room, and wherein the water-in of chamber 1 connects the hydrogen chloride synthetic furnace chuck, and water outlet is connected with gas-liquid heat exchanger by overflow spout; The water-in of chamber 2 connects the trichlorosilane synthetic furnace chuck, and water outlet connects the rectifying tower chuck, and device for storing liquid is connected with chamber 2 by the fluid infusion pipeline in addition.
7. method according to claim 6 is characterized in that: described chamber 1 is 1 with the volume ratio of chamber 2: 2-2: 1.
8. method according to claim 7 is characterized in that: described chamber 1 is 2 with the volume ratio of chamber 2: 3-4: 3.
9. method according to claim 8 is characterized in that: described chamber 1 is 5: 7 with the volume ratio of chamber 2.
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| CN2010106019253A CN102009979B (en) | 2010-12-23 | 2010-12-23 | Method for performing rectification and purification on trichlorosilane by using circulating heat |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006029930A1 (en) * | 2004-09-17 | 2006-03-23 | Degussa Ag | Apparatus and process for preparing silanes |
| CN101125654A (en) * | 2007-09-04 | 2008-02-20 | 浙江开化合成材料有限公司 | Large-scale fluidized bed reactor used for trichlorosilane production |
| CN101279735A (en) * | 2008-05-30 | 2008-10-08 | 中蓝晨光化工研究院有限公司 | Production method and apparatus for trichlorosilane |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006029930A1 (en) * | 2004-09-17 | 2006-03-23 | Degussa Ag | Apparatus and process for preparing silanes |
| CN101125654A (en) * | 2007-09-04 | 2008-02-20 | 浙江开化合成材料有限公司 | Large-scale fluidized bed reactor used for trichlorosilane production |
| CN101279735A (en) * | 2008-05-30 | 2008-10-08 | 中蓝晨光化工研究院有限公司 | Production method and apparatus for trichlorosilane |
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