CN203959830U - Prepare the system of polysilicon and the system of purify trichlorosilane - Google Patents
Prepare the system of polysilicon and the system of purify trichlorosilane Download PDFInfo
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- CN203959830U CN203959830U CN201420312266.5U CN201420312266U CN203959830U CN 203959830 U CN203959830 U CN 203959830U CN 201420312266 U CN201420312266 U CN 201420312266U CN 203959830 U CN203959830 U CN 203959830U
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Abstract
The utility model proposes and prepare the system of polysilicon and the system of purify trichlorosilane.Wherein, the system of preparing polysilicon comprises: hydrogen heating unit, trichlorosilane heating unit, reduction furnace, gas-liquid heat exchanger, hot water mixing device, trichlorosilane purification devices, the material inlet of reduction furnace is connected with trichlorosilane heating unit with hydrogen heating unit; Gas-liquid exchange device is connected with the cooling water outlet of trichlorosilane heating unit and the outlet of the tail gas of reduction furnace with hydrogen heating unit respectively; The water-in of hot water mixing device is connected with water-cooled assembly and the gas-liquid heat exchanger of reduction furnace respectively; And trichlorosilane purification devices comprises rectifying tower, and the thermal source import of rectifying tower is connected with the reduction workshop section hot water outlet of hot water mixing device, and the thermal source outlet of rectifying tower is connected with trichlorosilane heating unit and water-cooled assembly with hydrogen heating unit.Utilize said system can realize the recycle of water resources and heat energy, and then significantly save energy consumption.
Description
Technical field
The utility model relates to field polysilicon, and particularly, the utility model relates to prepares the system of polysilicon and the system of purify trichlorosilane.
Background technology
In existing production of polysilicon, especially in the preparation of polysilicon and the purifying technique of trichlorosilane, all need a large amount of water resourcess, thermal source and low-temperature receiver, cause the production of polysilicon to have the defect that energy consumption is good, cost is high.Therefore, existing relevant production of polysilicon technique still needs further improvement.
Utility model content
The utility model is intended to solve at least to a certain extent one of technical problem in correlation technique.For this reason, an object of the present utility model is to propose a kind of system of polysilicon and a kind of system of purify trichlorosilane prepared, utilize above-mentioned two kinds of systems to mate with thermal source in purify trichlorosilane preparing the reduction furnace water coolant and the heating raw materials water that use in polysilicon, and then make full use of water resources and save energy consumption.
According to an aspect of the present utility model, the system of preparing polysilicon of the utility model embodiment comprises:
Hydrogen heating unit, described hydrogen heating unit has hydrogen inlet, hydrogen outlet, hot water inlet and cooling water outlet;
Trichlorosilane heating unit, described trichlorosilane heating unit has trichlorosilane import, trichlorosilane outlet, hot water inlet and cooling water outlet;
Reduction furnace, described reduction furnace has reduction chamber and water-cooled assembly, and described reduction chamber has material inlet, products export and tail gas outlet, and described water-cooled assembly has entrance of cooling water and hot water outlet, wherein, outlet is connected described material inlet with trichlorosilane with described hydrogen outlet;
Gas-liquid heat exchanger, described gas-liquid exchange device is connected with the cooling water outlet of trichlorosilane heating unit and the outlet of the tail gas of reduction furnace with described hydrogen heating unit respectively;
Hot water mixing device, described hot water mixing device has water-in and reduction workshop section hot water outlet, and described water-in is connected with the hot water outlet of described water-cooled assembly and the hot water outlet of gas-liquid heat exchanger respectively; And
Trichlorosilane purification devices, described trichlorosilane purification devices comprises rectifying tower, and the thermal source import of described rectifying tower is connected with the reduction workshop section hot water outlet of described hot water mixing device, the thermal source outlet of described rectifying tower is connected with described hydrogen heating unit and the hot water inlet of trichlorosilane heating unit and the entrance of cooling water of described water-cooled assembly.
In addition, can also there is following additional technical characterictic according to the method for preparing polysilicon of the utility model above-described embodiment:
In the utility model, the above-mentioned system of preparing polysilicon further comprises:
Gas gas heat exchanger, described gas gas heat exchanger is connected with described hydrogen outlet, trichlorosilane outlet, tail gas outlet and gas-liquid heat exchanger respectively.
In the utility model, the above-mentioned system of preparing polysilicon further comprises:
Supplementary feed device, described supplementary feed device is connected with described hot water mixing device;
Heating unit, described heating unit is arranged between described hot water mixing device and described trichlorosilane purification devices.
In embodiment more of the present utility model, stating the system of preparing polysilicon further comprises: refrigerating unit, described refrigerating unit is arranged between described hot water mixing device and hydrogen heating unit, trichlorosilane heating unit and reduction furnace, and is connected with described reduction workshop section hot water outlet, hydrogen heating unit and the hot water inlet of trichlorosilane heating unit and the cooling water inlet of water-cooled assembly respectively.
In the utility model, described supplementary feed device further comprises:
Constant pressure tank, described Constant pressure tank is connected with described hot water mixing device;
Constant pressure tank;
Constant pressure pump, described constant pressure pump is arranged between described Constant pressure tank and described constant pressure tank;
Tensimeter, described tensimeter is connected with described Constant pressure tank and is arranged on a side of the water outlet of proximity thermal water mixing device.
According on the other hand of the present utility model, the utility model has also proposed a kind of system of purify trichlorosilane, contains dichloro-dihydro silicon and silicon tetrachloride in described trichlorosilane, it is characterized in that, the system of described purify trichlorosilane comprises:
The first rectification cell, described the first rectification cell has the first rectifying opening for feed, gas outlet and the first liquid heavy constituent outlet after liquid outlet, the first condensation after trichlorosilane outlet, the first condensation;
The second rectifier unit, described the second rectifier unit has gas outlet and the second liquid heavy constituent outlet after liquid outlet, the second condensation after the second rectifying opening for feed, the second condensation, and described the second rectifying opening for feed is connected with described the first liquid heavy constituent outlet;
Condensing works, described condensing works has gas outlet after liquid outlet and the 3rd condensation after phlegma import, the 3rd condensation, and described phlegma import exports and is connected with gas after gas outlet and the second condensation after described the first condensation; And
The 3rd rectifier unit, described the 3rd rectifier unit has gas outlet and the 3rd liquid heavy constituent outlet after liquid outlet, the 4th condensation after the 3rd rectifying opening for feed, the 4th condensation, described the 3rd rectifying opening for feed exports and is connected with liquid after liquid outlet after described the first condensation and described the 3rd condensation
Wherein, one of being at least connected with the system of preparing polysilicon of described the first rectification cell, the second rectifier unit, the 3rd rectifier unit, the described system of preparing polysilicon comprises:
Hydrogen heating unit, described hydrogen heating unit has hydrogen inlet, hydrogen outlet, hot water inlet and cooling water outlet;
Trichlorosilane heating unit, described trichlorosilane heating unit has trichlorosilane import, trichlorosilane outlet, hot water inlet and cooling water outlet;
Reduction furnace, described reduction furnace has reduction chamber and water-cooled assembly, and described reduction chamber has material inlet, products export and tail gas outlet, and described water-cooled assembly has entrance of cooling water and hot water outlet, wherein, outlet is connected described material inlet with trichlorosilane with described hydrogen outlet;
Gas-liquid heat exchanger, described gas-liquid exchange device is connected with the cooling water outlet of trichlorosilane heating unit and the outlet of the tail gas of reduction furnace with described hydrogen heating unit respectively; And
Hot water mixing device, described hot water mixing device has water-in and reduction workshop section hot water outlet, and described water-in is connected with the hot water outlet of described water-cooled assembly and the hot water outlet of gas-liquid heat exchanger respectively;
Wherein, one of being at least connected of the reduction workshop section hot water outlet of described hot water mixing device and described the first rectification cell, the second rectifier unit, the 3rd rectifier unit.
Brief description of the drawings
Fig. 1 is according to the structural representation of the system of preparing polysilicon of an embodiment of the utility model.
Fig. 2 is according to the structural representation of the system of preparing polysilicon of another embodiment of the utility model.
Fig. 3 is according to the structural representation of the system of preparing polysilicon of another embodiment of the utility model.
Fig. 4 is according to the structural representation of the system of the purify trichlorosilane of an embodiment of the utility model.
Fig. 5 utilizes the system of preparing polysilicon of an embodiment of the utility model to prepare the schema of the method for polysilicon.
Fig. 6 utilizes the system of preparing polysilicon of another embodiment of the utility model to prepare the schema of the method for polysilicon.
Embodiment
Describe embodiment of the present utility model below in detail, the example of described embodiment is shown in the drawings, and wherein same or similar label represents same or similar element or has the element of identical or similar functions from start to finish.Be exemplary below by the embodiment being described with reference to the drawings, be intended to for explaining the utility model, and can not be interpreted as restriction of the present utility model.
According to another aspect of the present utility model, the utility model has also proposed a kind of system of preparing polysilicon, describes the system of preparing polysilicon of the utility model embodiment below with reference to Fig. 1 in detail.
As shown in Figure 1, the system of preparing polysilicon of the utility model embodiment comprises: hydrogen heating unit 100, trichlorosilane heating unit 200, reduction furnace 300, gas-liquid heat exchanger 400, hot water mixing device 500 and trichlorosilane purification devices 600.
Wherein, hydrogen heating unit 100 has hydrogen inlet 110, hydrogen outlet 120, hot water inlet 130 and cooling water outlet 140;
Trichlorosilane heating unit 200 has trichlorosilane import 210, trichlorosilane outlet 220, hot water inlet 230 and cooling water outlet 240;
Reduction furnace 300 has reduction chamber and water-cooled assembly, described reduction chamber has material inlet 310, products export 320 and tail gas outlet 330, water-cooled assembly has entrance of cooling water 340 and hot water outlet 350, and wherein, material inlet 310 is connected with trichlorosilane outlet 220 with hydrogen outlet 120;
Gas-liquid exchange device 400 is connected with 240 and the tail gas outlet 330 of reduction furnace with the cooling water outlet 140 of hydrogen heating unit 100 and trichlorosilane heating unit 200 respectively;
Hot water mixing device 500 has water-in 510 and reduction workshop section hot water outlet 520, and water-in 510 is connected with the hot water outlet 350 of water-cooled assembly and the hot water outlet 410 of gas-liquid heat exchanger respectively; And
Trichlorosilane purification devices 600 comprises rectifying tower, and the thermal source import 610 of rectifying tower is connected with the reduction workshop section hot water outlet 520 of hot water mixing device, the hot water inlet 130 of the outlet 620 of the thermal source of rectifying tower and hydrogen heating unit and trichlorosilane heating unit is connected with 230 and the entrance of cooling water 340 of water-cooled assembly.
Commonly in the production of polysilicon, need a large amount of water resourcess, the hot water for example raw hydrogen and trichlorosilane being heated, reduction furnace is carried out cooling water coolant and needs a large amount of thermals source to the trichlorosilane purification of boiling again, therefore contriver of the present utility model finds, if by the recycle of mating by heat and the water yield between the water required purification of water and trichlorosilane in the preparation process of polysilicon, not only can save a large amount of water resourcess, can also save extra cooling and heating energy consumption simultaneously.But the number of opening or moving due to reduction furnace can change constantly, and the number of purify trichlorosilane rectifying tower used is unstable, be difficult to meet institute's water requirement and water temperature in two techniques, therefore the water in two techniques recycled to tool great difficulty.
Thus, the utility model is by designing the above-mentioned system of preparing polysilicon, can using the reduction workshop section hot water finally obtaining for trichlorosilane purification devices 600 the thermal source purify trichlorosilane as rectifying tower.Can significantly save thus water resources and energy consumption.In addition, by adopting the above-mentioned system of preparing polysilicon can realize recycle and the heat energy coupling of water resources.Particularly, the above-mentioned system of preparing polysilicon is to be implemented and realized circulation and the heat energy coupling of water resources by following manner.First hydrogen heating unit 100, trichlorosilane heating unit 200, reduction furnace 300 adopts respectively the water of 130 degrees Celsius carry out reduction reaction heating raw materials and carry out cooling to reduction furnace, be finally the reduction workshop section hot water of 150 degrees Celsius in the interior temperature that can obtain of hot water mixing device 500, further the reduction workshop section hot water of 150 degrees Celsius is used for to the thermal source purify trichlorosilane of trichlorosilane purification devices 600 as rectifying tower, and to obtain temperature be that the purification workshop section of 130 degrees Celsius returns to water, and returning to water, the purification workshop section that this temperature is 130 degrees Celsius just in time can return to hydrogen heating unit 100, trichlorosilane heating unit 200, in reduction furnace 300.By adopting the system of preparing polysilicon of the utility model above-described embodiment can realize water cycle and heat energy coupling, significantly save energy consumption thus.
As shown in Figure 2, also further comprise according to the system of preparing polysilicon of the utility model embodiment: gas gas heat exchanger 410, gas gas heat exchanger 410 is connected with hydrogen outlet 120, trichlorosilane outlet 220, tail gas outlet 330 and gas-liquid heat exchanger 400 respectively.
It is 110 degrees Celsius through the hydrogen of heat treated and the temperature of trichlorosilane, to before obtaining being incorporated into reduction furnace 300 through the hydrogen of heat treated and trichlorosilane, adopt in advance reduction tail gas to be preheated to 180 degrees Celsius.Thus the heat energy of reduction tail gas is made full use of and improves reduction reaction efficiency.
According to specific embodiment of the utility model, the above-mentioned system of preparing polysilicon further comprises: supplementary feed device 700 and heating unit 800, supplementary feed device 700 is connected with hot water mixing device 500, to add supplementary feed in reduction workshop section hot water.Heating unit 800 is arranged between hot water mixing device 500 and trichlorosilane purification devices 600.So that after adding reduction workshop section hot water heating to 150 after supplementary feed degree Celsius and as the thermal source of rectifying tower.Can ensure thus in the time that the water yield of reduction workshop section hot water can not meet in purifying technique institute's water consumption the water yield lacking to supply in reduction workshop section hot water in time.
As shown in Figure 3, according to specific embodiment of the utility model, above-mentioned supplementary feed device 700 further comprises: Constant pressure tank 710, constant pressure tank 720, constant pressure pump 730 and tensimeter 740, and wherein, Constant pressure tank 710 is connected with hot water mixing device 500; Constant pressure pump 730 is arranged between Constant pressure tank 710 and constant pressure tank 720; Tensimeter 740 is connected with Constant pressure tank 710 and cuts a side of the water outlet that is arranged on proximity thermal water mixing device 500.Can adopt thus tensimeter 740 to monitor constantly the pressure of the water between reduction workshop section's hot water and purification workshop section, and then judge that whether the water yield is not enough.Simultaneously tensimeter 740 with determine power pump 730 and constant pressure tank 720 is connected, and then according to supplementary feed in the automatic thermotropism water mixing device 500 of tensimeter 740 pressure changing.Can avoid thus, because service discharge deficiency causes the rectifying tower fluctuation of trichlorosilane purification devices 600 large, affecting quality product.
Therefore, according to specific embodiment of the utility model, the above-mentioned system of preparing polysilicon can further include: refrigerating unit 900, refrigerating unit arranges 900 between hot water mixing device 500 and hydrogen heating unit 100, trichlorosilane heating unit 200 and reduction furnace 300, and is connected with 230 and the cooling water inlet 340 of water-cooled assembly with the hot water inlet 130 of reduction workshop section hot water outlet 520, hydrogen heating unit and trichlorosilane heating unit respectively.The first part of reduction workshop section hot water can be used for to purify trichlorosilane as the thermal source of rectifying tower thus, the workshop section that simultaneously obtains purifying returns to water; And the second section of reduction workshop section hot water is carried out after cooling reducing the Part III of workshop section's hot water and purification workshop section and returning to one of at least mixing of water with being selected from, be the supplementary feed of 130 degrees Celsius to obtain temperature.
According to specific embodiment of the utility model, in the time of hot water amount described in the amount of the reduction workshop section hot water that hot water mixing device 500 provides has exceeded trichlorosilane purification devices 600, the system of preparing polysilicon of the utility model above-described embodiment can also be by adopting lower array apparatus to reach the coupling of the water yield.According to specific embodiment of the utility model, refrigerating unit 900 is connected with hot water mixing device 500, hydrogen heating unit 100, trichlorosilane heating unit 200 and reduction furnace 300, so that the thermal source using the first part of reduction workshop section hot water as rectifying tower is for purify trichlorosilane, the workshop section that simultaneously obtains purifying returns to water; The second section of reduction workshop section hot water is carried out after cooling reducing the Part III of workshop section's hot water and purification workshop section and returning to one of at least mixing of water with being selected from, and is the water of 130 degrees Celsius to obtain temperature; And be that the water of 130 degrees Celsius is for respectively to hydrogen with trichlorosilane heats and reduction furnace is carried out to water-cooled by obtained temperature.
Thus, obtaining the water of 130 degrees Celsius after the water of redundance can being lowered the temperature by refrigerating unit 900 again returns to water with purification workshop section to return to hydrogen heating unit 100, trichlorosilane heating unit 200 and reduction furnace 300 cooling for heating and the reduction furnace of raw material.And the utility model by the sub-fraction of reduction workshop section hot water unnecessary in hot water mixing device 500 is carried out cooling after and another part be mixed to get the water of 130 degrees Celsius, and then can save cooling energy consumption.
By adopting the system of preparing polysilicon of above-described embodiment of the present utility model, when the hot water amount of reduction workshop section in hot water mixing device 500 and trichlorosilane purification devices 600 rectifying tower institute water requirements are when identical, only need in advance hydrogen heating unit 100, trichlorosilane heating unit 200 and the required water of reduction furnace 300 be heated to after 130 degrees Celsius, the heat that makes full use of reduction tail gas in follow-up working cycle can arrive whole process water circulation, without extra heat, cold and extra supplementary feed.Can significantly save thus the water yield and energy consumption.
By adopting the system of preparing polysilicon of above-described embodiment of the present utility model, in the time that the hot water amount of reduction workshop section in hot water mixing device 500 is less than trichlorosilane purification devices 600 rectifying tower institute water requirement, can tensimeter 740 monitor force by device for supplying 700 change after automatically adding supplementary feed in the reduction workshop section hot water of thermotropism water mixing devices 500 and utilize heating unit 800 to be heated to approximately 150 degrees Celsius, and then avoid affecting not due to water shortage or temperature the quality product of trichlorosilane purification devices 600.
By adopting the system of preparing polysilicon of above-described embodiment of the present utility model, when the hot water amount of reduction workshop section in hot water mixing device 500 is when with trichlorosilane purification devices 600 rectifying tower institute water requirement, unnecessary hot water can be divided into two portions, utilize refrigerating unit 900 to carry out a part wherein cooling, and then be again delivered in hydrogen heating unit 100, trichlorosilane heating unit 200 and reduction furnace 300 after making unnecessary hot water temperature be down to 130 degrees Celsius.
The method for the preparation of polysilicon by the system of preparing polysilicon of the utility model above-described embodiment is described below, and the method specifically comprises the following steps:
(1) utilize hot water respectively hydrogen and trichlorosilane to be heated in hydrogen heating unit 100 and trichlorosilane heating unit 200, to obtain hydrogen and trichlorosilane through overcooled hot water and process heat treated,
(2) make the hydrogen of the process heat treated obtaining in step (1) and trichlorosilane in the interior generation reduction reaction of reduction furnace 300 more, to obtain polysilicon and reduction tail gas, wherein, in reduction reaction process, reduction furnace is carried out to water-cooled, and obtain the first hot water;
(3) utilize reduction tail gas to heating through overcooled hot water of obtaining in step (1), to obtain the second hot water; And
(4) the first hot water and described the second hot water are mixed, to obtain reducing workshop section's hot water, and reduction workshop section hot water is used for to purify trichlorosilane as the thermal source of rectifying tower, so that the workshop section that obtains purifying returns to water;
Wherein, the temperature of the first hot water and the second hot water is respectively independently within the scope of 145～155 degrees Celsius.
Commonly in the production of polysilicon, need a large amount of water resourcess, the hot water for example raw hydrogen and trichlorosilane being heated, reduction furnace is carried out cooling water coolant and needs a large amount of thermals source to the trichlorosilane purification of boiling again, therefore contriver of the present utility model finds, if by the recycle of mating by heat and the water yield between the water required purification of water and trichlorosilane in the preparation process of polysilicon, not only can save a large amount of water resourcess, can also save extra cooling and heating energy consumption simultaneously.But the number of opening or moving due to reduction furnace can change constantly, and the number of purify trichlorosilane rectifying tower used is unstable, be difficult to meet institute's water requirement and water temperature in two techniques, therefore the water in two techniques recycled to tool great difficulty.
According to embodiment of the present utility model, the hot water temperature who adopts in above-mentioned steps (1) is 130 degrees Celsius, and the chassis to reduction furnace and chuck carry out described water-cooled respectively in step (2), to adopt the water of 130 degrees Celsius.That is to say that preparing the needed water temp of polysilicon all can be 130 degrees Celsius, and the temperature of the reduction workshop section hot water obtaining after heating and water-cooled is 145～155 degrees Celsius, and the hot water of this temperature can be further used as rectifying tower thermal source for purify trichlorosilane.Contriver also finds, the temperature that the purification workshop section obtaining after heating rectifying tower returns to water is about 130 degrees Celsius, is just being used on the heat treated of the cooling and raw material of the reduction furnace of reduction reaction, thereby reached hot water temperature's coupling.Contriver of the present utility model has found above-mentioned two temperature just, can be about 150 degrees Celsius for rectifying tower heating with hot water, to rectifying tower temperature after heating near 130 degrees Celsius, further return for the preparation of polysilicon, utilize reduction tail gas further the water of reduction workshop section to be heated and finally obtains 150 degrees Celsius of water again for purify trichlorosilane, and then reach the coupling of water temp.
According to specific embodiment of the utility model, it is 110 degrees Celsius through the hydrogen of heat treated and the temperature of trichlorosilane, and before the hydrogen of the process heat treated obtaining in step (1) and trichlorosilane are incorporated into reduction furnace, adopt in advance reduction tail gas to be preheated to 180 degrees Celsius.Can make full use of thus the heat energy of reduction tail gas, improve the efficiency of reduction reaction.According to specific embodiment of the utility model, after first reduction tail gas heat hydrogen and trichlorosilane, further to above-mentioned carrying out preheating and then obtaining the hot water that temperature is about 150 degrees Celsius through overcooled hot water after hydrogen and trichlorosilane are heated.The heat energy of the utility model by making full use of reduction tail gas, by the hot water heating of reduction workshop section to being about 150 degrees Celsius, and then is applicable to purify trichlorosilane thus, provides guarantee for preparing polysilicon process water cycle.
According to specific embodiment of the utility model, in above-mentioned steps (4), can further include: supplementary feed and reduction workshop section hot water are mixed, and obtained mixing water is heated to the thermal source as rectifying tower after 150 degrees Celsius.Can ensure thus in the time that the water yield of reduction workshop section hot water can not meet in purifying technique institute's water consumption the water yield lacking to supply in reduction workshop section hot water in time.According to specific embodiment of the utility model, can adopt tensimeter to monitor constantly the pressure of the water between reduction workshop section's hot water and purification workshop section, and then judge that whether the water yield is not enough.Simultaneously tensimeter with determine power pump and constant pressure tank and be connected, and then according to tensimeter pressure changing supplementary feed in trend is reduced workshop section's hot water.Can avoid thus, because service discharge deficiency causes fluctuating greatly for the rectifying tower of purify trichlorosilane, affecting quality product.
According to specific embodiment of the utility model, first above-mentioned supplementary feed obtains through the following steps:
(4-1) thermal source using a part for reduction workshop section hot water as rectifying tower is for purify trichlorosilane, and the workshop section that simultaneously obtains purifying returns to water, and
(4-2) second section of described reduction workshop section hot water being carried out after water-cooled mixing with at least a portion that is selected from the described Part III that reduces workshop section's hot water and described purification workshop section and returns water, is the described supplementary feed of 130 degrees Celsius to obtain temperature.
According to specific embodiment of the utility model, in the time of hot water amount described in the amount of reduction workshop section hot water has exceeded purify trichlorosilane, the method for preparing polysilicon of the utility model above-described embodiment can also reach the coupling of the water yield through the following steps.According to specific embodiment of the utility model, in above-mentioned steps (4), can further include:
(4-1) thermal source using the first part of reduction workshop section hot water as rectifying tower is for purify trichlorosilane, and the workshop section that simultaneously obtains purifying returns to water;
(4-2) second section of reduction workshop section hot water being carried out after water-cooled reducing at least a portion that the Part III of workshop section's hot water and purification workshop section return to water and mixing with being selected from, is the water of 130 degrees Celsius to obtain temperature.
Thus, again return to water with purification workshop section and return to and heating raw material cooling for reduction furnace by obtaining the water of 130 degrees Celsius after the water of redundance is lowered the temperature.And the utility model by the sub-fraction of unnecessary reduction workshop section hot water is carried out cooling after and another part be mixed to get the water of 130 degrees Celsius, and then can save cooling energy consumption.
By adopting the method for preparing polysilicon of above-described embodiment of the present utility model, in the time that the reduction hot water amount of workshop section is identical with the purification workshop section water yield, only need in advance this water be heated to after 130 degrees Celsius, the heat that only need to make full use of reduction tail gas in follow-up working cycle can arrive whole process water circulation, without extra heat, cold and extra supplementary feed.Can significantly save thus the water yield and energy consumption.
By adopting the method for preparing polysilicon of above-described embodiment of the present utility model, in the time that the reduction workshop section hot water water yield is less than the purification workshop section water yield, can change after automatically adding supplementary feed in reduction workshop section hot water and again be heated to approximately 150 degrees Celsius by monitor force, and then avoid affecting the quality of purification workshop section trichlorosilane.
By adopting the method for preparing polysilicon of above-described embodiment of the present utility model, when the reduction workshop section water yield is when with the purification workshop section water yield, by unnecessary hot water is divided into two portions, a part is wherein carried out cooling, and then after making unnecessary hot water temperature be down to 130 degrees Celsius again for reducing workshop section.
The utility model proposes a kind of system of purify trichlorosilane more on the one hand according to of the present utility model, wherein trichlorosilane contains dichloro-dihydro silicon and silicon tetrachloride, as shown in Figure 4, comprises according to the system of the purify trichlorosilane of the utility model embodiment:
The first rectification cell 100: according to embodiment of the present utility model, the first rectification cell 100 has gas outlet 104 and the first liquid heavy constituent outlet 105 after liquid outlet 103 after the first rectifying opening for feed 101, trichlorosilane outlet 102, the first condensation, the first condensation, be suitable for chlorosilane to carry out the first rectification process, thereby can obtain respectively gas and the first liquid heavy constituent after liquid after trichlorosilane, the first condensation, the first condensation.According to embodiment of the present utility model, after the first condensation, liquid can contain dichloro-dihydro silicon and trichlorosilane, and the first liquid heavy constituent can contain silicon tetrachloride and trichlorosilane.According to embodiment of the present utility model, can adopt the rectifying tower of multiple series connection to carry out the first rectification process, according to specific embodiment of the utility model, can adopt the rectifying tower of five series connection to carry out the first rectification process.According to concrete example of the present utility model, the rectifying tower of five series connection comprises the first to the 5th rectifying tower, and each includes: liquid outlet at the bottom of tower body, overhead gas outlet, tower, opening for feed, condensation separator, well heater, wherein, in tower body, limit rectifying space, be suitable for the material in rectifying space to carry out rectification process, thereby can obtain respectively liquid and overhead gas at the bottom of tower; Overhead gas outlet is arranged on the top of tower body, is suitable for exporting overhead gas; At the bottom of tower, liquid outlet is arranged on the bottom of tower body, is suitable for exporting liquid at the bottom of tower; Opening for feed is arranged on tower body, is suitable for introducing the material for the treatment of rectifying in rectifying space; Condensation separator is connected with overhead gas outlet, is suitable for overhead gas to carry out condensation separation processing, thereby can obtains condensing air and phlegma; Well heater is connected with tower body, is suitable for rectifying space to heat.
According to embodiment of the present utility model, by second to one of being at least connected with the opening for feed of the first rectifying tower of liquid outlet at the bottom of the tower of the 5th rectifying tower, to make liquid at the bottom of tower that the second to the 5th rectifying tower one of at least discharges treat the use of rectifying material as the first rectifying tower.For example, can return as the treating rectifying material of the first rectifying tower and use using the 4th to liquid at the bottom of the tower of the 5th rectifying tower.Particularly, at the bottom of tower, in liquid, contain the trichlorosilane of part, by liquid at the bottom of tower is returned and proceeds rectification process, can significantly improve the utilization ratio of material.
The second rectifier unit 200: according to embodiment of the present utility model, the second rectifier unit 200 has gas outlet 203 and the second liquid heavy constituent outlet 204 after liquid outlet 102, the second condensation after the second rectifying opening for feed 201, the second condensation, wherein, the second rectifying opening for feed 201 is connected with the first liquid heavy constituent outlet 105, be suitable for the liquid heavy constituent of above gained first to carry out the second rectification process, thereby can obtain gas and the second liquid heavy constituent after liquid after the second condensation, the second condensation.According to embodiment of the present utility model, after the second condensation, in liquid, contain silicon tetrachloride.According to specific embodiment of the utility model, at the bottom of the first to the 5th rectifying tower tower one of at least, liquid outlet is connected with the second rectifying opening for feed 201 of the second rectifier unit 200, for liquid at the bottom of the first to the 5th rectifying tower tower one of is at least carried out to the second rectification process, for example, liquid outlet at the bottom of the tower of Second distillation column can be connected with the second rectifying opening for feed 201 of the second rectifier unit 200, carry out the second rectification process for liquid at the bottom of Second distillation column tower as the first liquid heavy constituent.According to embodiment of the present utility model, the second liquid restructuring is divided into waste liquid, can directly be delivered to liquid waste disposal operation and process.Contriver finds, contains silicon tetrachloride and a large amount of heavy constituent impurity at the bottom of Second distillation column tower in liquid, can effectively remove most heavy constituent impurity, thereby can obtain finished product silicon tetrachloride by carrying out the second rectification process.Particularly, the second rectifier unit can be high-efficiency guide sieve-plate tower, tower internal diameter is 2200mm, stage number is 60, and opening for feed is 25th～45 blocks of column plates, and tower top working pressure is 0.213MPaG, service temperature is 89～92 DEG C, tower reactor working pressure is 0.223MPaG, and service temperature is 128～131 DEG C, and reflux ratio is 4.5.
Condensing works 300: according to embodiment of the present utility model, condensing works 300 put there is phlegma import 301, gas outlet 303 after liquid outlet 302 and the 3rd condensation after the 3rd condensation, wherein, phlegma import 301 and gas outlet after the first condensation 104 are connected with gas outlet 203 after the second condensation, for to gas after gas and the second condensation after above gained the first condensation one of at least carry out condensation process, thereby can obtain after the 3rd condensation gas after liquid and the 3rd condensation.According to embodiment of the present utility model, the condition of condensation process is also not particularly limited, and according to specific embodiment of the utility model, condensation process can be to carry out under-40～-38 degrees Celsius and the pressure condition that is 0.1～0.15MPaG in temperature.Contriver finds, the condensation process of carrying out under this condition can obviously improve after condensation the separation efficiency of liquid after gas and condensation.According to embodiment of the present utility model, after the condensation one of at least producing that can the using first to the 5th rectifying tower, gas gas after the first condensation carries out condensation process.Contriver finds, contains a large amount of dichloro-dihydro silicon and a small amount of trichlorosilane after the first condensation after gas and the second condensation in gas, is carried out carrying out subsequent disposal after condensation process again, can significantly improve the utilization ratio of material, can reduce exhaust emissions amount simultaneously.According to embodiment of the present utility model, after the 3rd condensation, in gas, contain noncondensable gas, can directly be sent to off gas treatment operation and process.According to specific embodiment of the utility model, condensing works can be double-tube sheet shell and tube heat exchanger, heat exchanger tube pass fluid is gas after each tower condensation, shell-side fluid is-38 DEG C of chilled brines, in upper cover, there is a pass partition, dividing plate one side has gas admission port after each tower condensation, and opposite side has noncondensable gas discharge outlet, and lower cover has a condensate discharge mouth.
The 3rd rectifier unit 400: according to embodiment of the present utility model, the 3rd rectifier unit 400 has gas outlet 403 and the 3rd liquid heavy constituent outlet 404 after liquid outlet 402, the 4th condensation after the 3rd rectifying opening for feed 401, the 4th condensation, wherein, the 3rd rectifying opening for feed 401 and liquid outlet after the first condensation 103 are connected with liquid outlet 302 after the 3rd condensation condensation, for to liquid after liquid after the first condensation and the 3rd condensation one of at least carry out the 3rd rectification process, thereby can obtain gas and the 3rd liquid heavy constituent after liquid after the 4th condensation, the 4th condensation.According to specific embodiment of the utility model, after the 4th condensation, in liquid, contain dichloro-dihydro silicon, the 3rd liquid heavy constituent contains trichlorosilane.According to embodiment of the present utility model, one of being at least connected with the 3rd rectifying discharge port 401 of the 3rd rectifier unit 400 of the first condensation separator to the 5th rectifying tower, be suitable for condensation that the using first to the 5th rectifying tower one of at least produces after liquid liquid after the first condensation carry out the 3rd rectification process.For example, can be connected with the condensation separator of the 3rd rectifying tower and the 3rd rectifying discharge port 401 of the 3rd rectifier unit 400 first, for by first and the 3rd after the condensation that produces of rectifying tower after liquid and the 3rd condensation liquid carry out the 3rd rectification process.Contriver finds, in the first and the 3rd liquid after rectifying tower condensation, contain more than 99% trichlorosilane, the dichloro-dihydro silicon less than 1% and a large amount of light constituent impurity (as the compound of boron), can remove most of dichloro-dihydro silicon and the lower-boiling impurity in light constituent material by the 3rd rectification process, and can reach more than 99.99% through trichlorosilane content in the 3rd rectification process gained the 3rd liquid heavy constituent.According to embodiment of the present utility model, the 3rd rectifier unit can be high-efficiency guide sieve-plate tower, tower internal diameter is 1200mm, stage number is 76, and opening for feed is 32nd～55 blocks of column plates, and tower top working pressure is 0.248MPaG, service temperature is 55～58 DEG C, tower reactor working pressure is 0.298MPaG, and service temperature is 77～79 DEG C, and reflux ratio is 47.
Can prepare the required trichlorosilane of electronic-grade polycrystalline silicon according to the system of purify trichlorosilane from chlorosilane of the utility model embodiment, and by gas centralized recovery after gas and the second condensation after the condensation that the first to the 5th rectifying tower is produced, and gas after condensation is concentrated and carried out condensation process, can obviously reduce the consumption of cold and the discharge of tail gas, liquid at the bottom of Second distillation column tower is proceeded to rectification process simultaneously, can obtain silicon tetrachloride product, in addition, after the condensation that the first to the 5th rectifying tower one of is at least produced, after liquid and the 3rd condensation, liquid is proceeded rectification process, can effectively trichlorosilane wherein be separated with dichloro-dihydro silicon.
According to specific embodiment of the utility model, one of being at least connected with the hot water mixing device 500 in the system of preparing polysilicon of above-described embodiment of above-mentioned the first rectification cell, the second rectifier unit, the 3rd rectifier unit, utilize thus reduction workshop section hot water to heat the first rectification cell, the second rectifier unit, the 3rd rectifier unit, the cold water of simultaneously discharging and the hot water inlet 130 of hydrogen heating unit 100 and trichlorosilane heating unit 200 are connected with 230 and the cooling water inlet 340 of water-cooled assembly.
Embodiment
With reference to figure 5-6, high temperature water inlet (24) after each rectifying tower system heat exchange is with 0.6MPaG, 130 DEG C to enter respectively each chassis of reducing furnace cooling, chuck is cooling, tail gas is cooling, the cooling water inlet in chassis (6) through with chassis of reducing furnace heat exchange after be heated to 150 DEG C, the cooling water inlet of chuck (4) through with the heat exchange of reduction furnace bell jar after be heated to 150 DEG C, the cooling water inlet of tail gas (1) and reduction furnace feeding trichlorosilane liquid (9) well heater (E1), hydrogen gas (8) well heater (E2) carries out heat exchange, trichlorosilane, hydrogen is vaporized through 130 DEG C of hot water heatings, mix by a certain percentage, form 110 DEG C of mixed gass (10), mixed gas (10) enters reduction furnace mixed gas preheater (E3), enter and in reduction furnace, carry out polysilicon deposition with 580 DEG C of-610 DEG C of reduction furnace tail gas (12) heat exchange gas mixture (11) that is 180 DEG C, after mixed gas well heater (E3) heat exchange, reduce tail gas (13), enter again reduction exhaust gas cooler (E4) and carry out heat exchange with the tail gas water coolant (2) of trichlorosilane, hydrogen heater outlet, by 100 DEG C of-110 DEG C of reduction furnace tail gas of heat exchange (14) to device for recovering tail gas,
(3) 140 DEG C-145 DEG C, tail gas water coolant backwater and chuck cooling backwater (5), chassis water coolant backwater (7) are mixed into reduction furnace high-temperature tempering house steward (25), boost to 1.0MPaG with pump (P2) and be sent to steam heater (E5), enter again the heat exchange of each rectifying tower reboiler, reduction furnace high-temperature tempering (22) and the heat exchange to 130 DEG C of each rectifying tower reboiler, after water recirculator (E6), (23) are returned to each reduction furnace and are carried out cooling heat transferring, recycle.
High-temperature water system adopts closed type, for making high-temperature water system pressure and stability of flow, between reduction furnace high-temperature water pipeline (23) and constant pressure pump (P1), increase a Constant pressure tank, on the pipeline being connected with reduction furnace high-temperature water, (17) increase tensimeter simultaneously, tensimeter will directly show jacket water (J.W.) system pressure, when system pressure is when arranging minimum pressure 0.97MPaG, tensimeter is by given transmission signal water pump (P1), level pressure water pump (P1) is started working, and by (14), high-temperature tempering pipeline (15) is carried out to supercharging; When system pressure is greater than when top pressure 1.05MPAG is set, tensimeter is by given transmission signal water pump (P1), and level pressure water pump (P1) quits work.After level pressure water pump (P1) quits work, high-temperature water system pressure compensates by Constant pressure tank, in the time of high-temperature water system pressure drop, gas in Constant pressure tank is wanted naturally to expand, and interior water automatically fills into high-temperature tempering pipeline (15) through (14) under gaseous tension; When the water in Constant pressure tank is reduced to a certain degree, realize supercharging by level pressure water pump, the gas in tank is again compressed.Work and so forth, high-temperature water system carries out voltage stabilizing and moisturizing.
Reduction furnace high-temperature tempering is as the direct heat source of rectifying tower system reboiler, reduction furnace start-stop can be to rectifying tower system temperature in process of production, flow causes fluctuation and the system system hot water temperature that drives for the first time not to reach rectifying tower reboiler temperature, flow, before entering rectifying tower system reboiler, reduction furnace high-temperature tempering (20) increases a steam heater (E5), steam (28) is with 1.2MPaG, 190 DEG C are heated to 150 DEG C by reduction steam heater (E5) by reduction furnace high-temperature tempering (20), reduction steam heater (E5) bottom steam water of condensation (29) is got back to boiler, high-temperature tempering house steward (23) and reduction high-temperature water house steward enter, going out bypass (15) regulates, make to enter rectifying tower system high-temperature water (21) temperature and stability of flow at 150 DEG C, 1700m
3/ h, has ensured that rectifying tower processing parameter is stable, rectifying tower system part is stopped tower to operation reduction furnace high temperature water inlet (23) temperature in process of production, flow can cause fluctuation, enter (17) at rectifying tower reboiler, return main (22) increases a set of recirculated water plate-type heat exchanger (E6), recirculated water enters (26), recirculated water water outlet (27) is undertaken cooling by recirculated water plate-type heat exchanger (E6) by high-temperature cooling water (19), enter steam heater (E5) reduction furnace high temperature water inlet manifold (17) bypass (18) to rectifying tower system water plate-type heat exchanger reboiler backwater (22) afterwards, rely on bypass (18) to regulate, ensure to enter reducing furnace system high temperature cooling water inlet (23) temperature, stability of flow is at 130 DEG C, 2100m
3/ h.
5000 tons/year of polycrystalline silicon production lines, reduction direct consumption of electr ic energy 70kw.h/kgsi, product 625kg silicon per hour, chuck, chassis, tail gas water coolant are taken away approximately 80% heat, the heat of reduction furnace chuck, chassis, the recovery per hour of tail gas water coolant: 35000KW.Reduction furnace chuck, chassis, tail gas water coolant by 130 DEG C of water inlets, 150 DEG C of water outlets, 20 DEG C of calculating of the temperature difference, the total Water needing: 35000*860.6/20=1506m
3/ h;
Distillation system amounts to 13 towers, and 6, synthetic material rectifying tower, reverts back 6, rewinding rectifying tower, 1, silicon tetrachloride rectifying tower, and the each tower reboiler of synthetic material rectifying tower institute thermal losses is 1870KW, the heat dissipation water 78m of institute
3/ h, reverting back the each tower reboiler of rewinding rectifying tower institute thermal losses is 3920KW, the heat dissipation water 164m of institute
3/ h, silicon tetrachloride rectifying tower reboiler institute thermal losses is 3950KW, the heat dissipation water 165m of institute
3/ h; It is 38690KW that rectifying tower system amounts to institute's thermal losses, the heat dissipation water 1617m of institute
3/ h;
After reduction furnace chuck, chassis, the comprehensive utilization of tail gas cooled water heat energy, whole distillation system only need to supplement 5.2t/h steam and can meet, reduction furnace high-temperature water does not need circulating water, distillation system does not need steam heating, can be rectifying tower system minimizing heat per hour 35000KW, amount to steam 50t/h, steam be by 140 yuan/ton of calculating, per hourly 7000 yuan can be saved, 5,040 ten thousand yuan can be saved the whole year.Reduction chuck, chassis, tail gas water coolant are pressed circulating water, 5 DEG C of temperature difference of recirculated water, and quantity of circulating water is exactly 35000X861.24 ÷ 5 ÷ 1000=6028m so
3/ h, a water circulating pump flow is 5000m
3/ h, a water circulating pump power is 1000kw.h, separate unit power of fan is 180kw.h, calculates by 0.5 yuan/kw.h: per hourly can save 590 yuan, can save 424.8 ten thousand yuan the whole year; Circulating water system year is saved moisturizing 100000m
3, every Fang Shui is by 5 yuan of calculating, and year is saved 500,000 yuan.
Three add up to save the whole year: ten thousand yuan of 5040+424.8+50=5514.8
The technology transformation can make distillation system reduce by 91% steam consumption, makes device for recovering tail gas reduce refrigerator load 5%, and reduction power consumption reduces by 10%, and full factory recirculated water consumption reduces approximately 33.4%.
In the description of this specification sheets, the description of reference term " embodiment ", " some embodiment ", " example ", " concrete example " or " some examples " etc. means to be contained at least one embodiment of the present utility model or example in conjunction with specific features, structure, material or the feature of this embodiment or example description.In this manual, to the schematic statement of above-mentioned term needn't for be identical embodiment or example.And, specific features, structure, material or the feature of description can one or more embodiment in office or example in suitable mode combination.In addition,, not conflicting in the situation that, those skilled in the art can carry out combination and combination by the feature of the different embodiment that describe in this specification sheets or example and different embodiment or example.
Although illustrated and described embodiment of the present utility model above, be understandable that, above-described embodiment is exemplary, can not be interpreted as restriction of the present utility model, those of ordinary skill in the art can change above-described embodiment in scope of the present utility model, amendment, replacement and modification.
Claims (6)
1. a system of preparing polysilicon, is characterized in that, comprising:
Hydrogen heating unit, described hydrogen heating unit has hydrogen inlet, hydrogen outlet, hot water inlet and cooling water outlet;
Trichlorosilane heating unit, described trichlorosilane heating unit has trichlorosilane import, trichlorosilane outlet, hot water inlet and cooling water outlet;
Reduction furnace, described reduction furnace has reduction chamber and water-cooled assembly, and described reduction chamber has material inlet, products export and tail gas outlet, and described water-cooled assembly has entrance of cooling water and hot water outlet, wherein, outlet is connected described material inlet with trichlorosilane with described hydrogen outlet;
Gas-liquid heat exchanger, described gas-liquid exchange device is connected with the cooling water outlet of trichlorosilane heating unit and the outlet of the tail gas of reduction furnace with described hydrogen heating unit respectively;
Hot water mixing device, described hot water mixing device has water-in and reduction workshop section hot water outlet, and described water-in is connected with the hot water outlet of described water-cooled assembly and the hot water outlet of gas-liquid heat exchanger respectively; And
Trichlorosilane purification devices, described trichlorosilane purification devices comprises rectifying tower, and the thermal source import of described rectifying tower is connected with the reduction workshop section hot water outlet of described hot water mixing device, the thermal source outlet of described rectifying tower is connected with described hydrogen heating unit and the hot water inlet of trichlorosilane heating unit and the entrance of cooling water of described water-cooled assembly.
2. the system of preparing polysilicon according to claim 1, is characterized in that, further comprises:
Gas gas heat exchanger, described gas gas heat exchanger is connected with described hydrogen outlet, trichlorosilane outlet, tail gas outlet and gas-liquid heat exchanger respectively.
3. the system of preparing polysilicon according to claim 2, is characterized in that, further comprises:
Supplementary feed device, described supplementary feed device is connected with described hot water mixing device;
Heating unit, described heating unit is arranged between described hot water mixing device and described trichlorosilane purification devices.
4. the system of preparing polysilicon according to claim 3, is characterized in that, further comprises:
Refrigerating unit, described refrigerating unit is arranged between described hot water mixing device and hydrogen heating unit, trichlorosilane heating unit and reduction furnace, and is connected with described reduction workshop section hot water outlet, hydrogen heating unit and the hot water inlet of trichlorosilane heating unit and the cooling water inlet of water-cooled assembly respectively.
5. the system of preparing polysilicon according to claim 4, is characterized in that, described supplementary feed device further comprises:
Constant pressure tank, described Constant pressure tank is connected with described hot water mixing device;
Constant pressure tank;
Constant pressure pump, described constant pressure pump is arranged between described Constant pressure tank and described constant pressure tank;
Tensimeter, described tensimeter is connected with described Constant pressure tank and is arranged on a side of the water outlet of contiguous described hot water mixing device.
6. a system for purify trichlorosilane, described chlorosilane contains dichloro-dihydro silicon, trichlorosilane and silicon tetrachloride, it is characterized in that, and the system of described purify trichlorosilane comprises:
The first rectification cell, described the first rectification cell has the first rectifying opening for feed, gas outlet and the first liquid heavy constituent outlet after liquid outlet, the first condensation after trichlorosilane outlet, the first condensation;
The second rectifier unit, described the second rectifier unit has gas outlet and the second liquid heavy constituent outlet after liquid outlet, the second condensation after the second rectifying opening for feed, the second condensation, and described the second rectifying opening for feed is connected with described the first liquid heavy constituent outlet;
Condensing works, described condensing works has gas outlet after liquid outlet and the 3rd condensation after phlegma import, the 3rd condensation, and described phlegma import exports and is connected with gas after gas outlet and the second condensation after described the first condensation; And
The 3rd rectifier unit, described the 3rd rectifier unit has gas outlet and the 3rd liquid heavy constituent outlet after liquid outlet, the 4th condensation after the 3rd rectifying opening for feed, the 4th condensation, described the 3rd rectifying opening for feed exports and is connected with liquid after liquid outlet after described the first condensation and described the 3rd condensation
Wherein, one of being at least connected with the system of preparing polysilicon of described the first rectification cell, the second rectifier unit, the 3rd rectifier unit, the described system of preparing polysilicon comprises:
Hydrogen heating unit, described hydrogen heating unit has hydrogen inlet, hydrogen outlet, hot water inlet and cooling water outlet;
Trichlorosilane heating unit, described trichlorosilane heating unit has trichlorosilane import, trichlorosilane outlet, hot water inlet and cooling water outlet;
Reduction furnace, described reduction furnace has reduction chamber and water-cooled assembly, and described reduction chamber has material inlet, products export and tail gas outlet, and described water-cooled assembly has entrance of cooling water and hot water outlet, wherein, outlet is connected described material inlet with trichlorosilane with described hydrogen outlet;
Gas-liquid heat exchanger, described gas-liquid exchange device is connected with the cooling water outlet of trichlorosilane heating unit and the outlet of the tail gas of reduction furnace with described hydrogen heating unit respectively; And
Hot water mixing device, described hot water mixing device has water-in and reduction workshop section hot water outlet, and described water-in is connected with the hot water outlet of described water-cooled assembly and the hot water outlet of gas-liquid heat exchanger respectively;
Wherein, one of being at least connected of the reduction workshop section hot water outlet of described hot water mixing device and described the first rectification cell, the second rectifier unit, the 3rd rectifier unit.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105066716A (en) * | 2015-07-28 | 2015-11-18 | 中国恩菲工程技术有限公司 | Waste heat recycling method of reduction furnace |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105066716A (en) * | 2015-07-28 | 2015-11-18 | 中国恩菲工程技术有限公司 | Waste heat recycling method of reduction furnace |
| CN105066716B (en) * | 2015-07-28 | 2018-02-02 | 中国恩菲工程技术有限公司 | The method that afterheat of reducing furnace recycles |
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