CN111646478B - Micro-negative pressure external refining method for industrial silicon melt - Google Patents
Micro-negative pressure external refining method for industrial silicon melt Download PDFInfo
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Abstract
The invention relates to a micro-negative pressure external refining method of industrial silicon melt, belonging to the technical field of fire refining and purification of silicon melt. The invention moves the micro negative pressure device to the position right above the ladle opening of the external refining device, opens the vacuum device of the micro negative pressure device to carry out micro negative pressure external refining on the industrial silicon melt, removes volatile impurities in the industrial silicon melt in the external refining process of the industrial silicon melt, and improves the quality of silicon products. The micro-negative pressure environment is created above the silicon melt, so that the escape of smoke in the external refining process of the silicon melt can be avoided, and the environmental influence is reduced. The method has the advantages of simple equipment requirement, easy operation, environmental protection and suitability for large-scale industrial production.
Description
Technical Field
The invention relates to a micro-negative pressure external refining method of industrial silicon melt, belonging to the technical field of industrial silicon smelting.
Background
In the process of producing and preparing industrial silicon by a submerged arc electric arc furnace, in order to further reduce the impurity content in the silicon melt, the silicon melt is required to be refined outside the furnace to prepare high-quality industrial silicon. In the external refining process, the refining means adopted aiming at different impurities mainly comprises blowing refining, slagging refining, oxidation refining and the like.
In the prior art, the conventional blowing refining, slagging refining and oxidation refining mainly remove impurities by utilizing the principle that aluminum and calcium impurities in silicon melt have high affinity with oxygen and are distributed in slag in a large proportion, and a large amount of industrial oxygen, air and slag agents are required to be consumed in the refining process, so that the energy input consumption and the emission of industrial three wastes are increased, and new requirements on the service life, the erosion resistance and the like of equipment in the actual production process, the equipment control operation level and the like are provided. The invention realizes the removal of the impurities by utilizing the property that the saturated vapor pressure of the impurities of aluminum and calcium is large and volatile under the condition of micro negative pressure, does not need to invest other energy consumption, has no special requirement on equipment use, has low production cost and is easy to realize industrial application.
Disclosure of Invention
The invention aims to provide a micro-negative pressure external refining method of industrial silicon melt, namely, a micro-negative pressure environment is created at the upper part of external refining, namely a gas-liquid interface of the refined silicon melt, through a micro-negative pressure device, the reaction speed is accelerated, the removal of volatile impurities is promoted, the loss of harmful substances of smoke and furnace dust in the refining process is reduced, and the efficient impurity removal and clean production in the silicon refining process are realized.
A micro negative pressure external refining method of industrial silicon melt comprises the following specific steps:
and moving the micro negative pressure device to be right above a ladle opening of the external refining device, and starting a vacuum device of the micro negative pressure device to carry out micro negative pressure external refining on the industrial silicon melt so as to remove volatile impurities in the industrial silicon melt.
The external refining comprises air blowing refining, slagging refining or air blowing-slagging composite refining;
further, the oxygen introducing mode can specifically adopt bottom blowing, top blowing, side blowing or eccentric blowing and the like aiming at different furnace types; the slag agent can be one or more of oxide, fluoride and fluoroaluminate; the gas can be air, wet oxygen, industrial oxygen or oxygen-enriched air, and can also be mixed gas containing argon, nitrogen and water; blowing in gas not only can play the effect of edulcoration, can also acutely stir silicon melt simultaneously, thereby make the gas-liquid interface of furnace mouth department constantly renew when guaranteeing impurity abundant and edulcoration agent reaction and more do benefit to volatile impurity and volatilize and get rid of.
The micro negative pressure device comprises a smoke collecting hood, a flue, a vacuum unit and a dust collecting device which are sequentially connected, wherein the smoke collecting hood is arranged right above a ladle port of the external refining device, and the smoke collecting hood is hermetically connected with the ladle port of the external refining device to form a sealed cavity.
Further, the outer wall of the exhaust fume collecting hood is connected with an overhead crane suspension or lifting-rotating component system.
Furthermore, the outer wall of the fume collecting hood is connected with a lifting-rotating component, the lifting-rotating component comprises a controller, a driving servo motor I and a driving servo motor II, the device comprises a transmission shaft I, a transmission shaft II and a clamping connecting rod, wherein one end of the clamping connecting rod is fixedly connected with the outer wall of the smoke collecting hood, the other end of the clamping connecting rod is fixedly connected with the top end of the transmission shaft I, the bottom end of the transmission shaft I is connected with the top end of the transmission shaft II through a ball bearing or a needle bearing, the transmission shaft I can rotate at the top end of the transmission shaft II, the bottom end of the transmission shaft II is fixedly connected with an output shaft of a driving servo motor II, the driving servo motor II is a stepping reciprocating motor, the driving servo motor I is fixedly arranged on the transmission shaft II through a supporting rod, a gear I is arranged on the output shaft of the driving servo motor I, a gear II is sleeved on the transmission shaft I, and the gear I and the gear II are positioned on the same horizontal plane and are in meshed transmission; the driving servo motor I and the driving servo motor II are respectively electrically connected with the controller (see figure 2).
Further, a fire-resistant layer and a cooling water jacket are arranged on the outer wall of the smoke collecting hood;
the top opening of the external refining device can be used for introducing gas from the top, adding a slagging agent and pouring slag and silicon liquid, smoke and dust fume generated in the refining process is generated at a gas-liquid interface and collected in a fume collecting hood under the action of micro negative pressure, the area of a fume collecting hood opening can cover the whole top opening of the external refining device, the lifting-rotating member of the fume collecting hood can be adjusted in height according to different refining periods, for example, the fume collecting hood can be properly lifted in the ventilation process and the slagging agent is added, and the fume collecting hood can be lifted to a specific height when the silicon liquid is added or discharged; the fire-resistant layer of the smoke collecting hood can ensure that the smoke collecting hood can bear different refining temperatures;
The secondary refining device can be a two-man ladle refining furnace, a tundish, a graphite crucible or other special refining equipment;
the heating mode of the external refining device comprises but is not limited to: resistance heating, induction heating, plasma, arc furnace heating, self-heating of reaction production or heat capacity of silicon melt, etc.;
the fume collecting hood can be in the shape of a round bottom, a conical shape, a tetrahedral frustum and the like, and the specific size and the cross section shape can be determined according to the geometric shape and the size of a top opening of a specific external refining device so as to ensure the complete connection between the fume collecting hood and a furnace opening, thereby avoiding the escape, the overflow, the leakage and the like of furnace gas and ensuring the micro negative pressure environment in the fume collecting hood;
the smoke collecting hood can be made of a stainless steel shell layer, a steel sleeve and the like, and the outer wall of the smoke collecting hood is lined with a fire-resistant layer and a cooling water jacket, so that the rigidity, the strength and the high temperature resistance of the smoke collecting hood are ensured, and the pollution of an external pollution source to the silicon melt is avoided;
the raw material of the industrial silicon melt is industrial silicon or secondary silicon-containing resources from different sources;
the vacuum equipment of the vacuum device is a one-stage or multi-stage combined vacuum pump, and the vacuum pump is a rough pumping mechanical pump or a molecular pump; the vacuum system can be determined according to the content and the type of impurities in silicon melts from different sources or in different batches, for example, a multistage vacuum pump can be adopted for silicon melts with higher volatile impurities to keep the furnace mouth at a relatively higher vacuum degree, so that the deep removal of a large amount of volatile impurities is ensured, and the refining period can be effectively shortened.
The dust collecting system can be a cloth bag, cyclone, gravity or electrostatic dust collecting equipment and can simultaneously collect micro silicon powder, silicon powder and the like carried in smoke dust in the refining process outside the furnace.
The beneficial effects of the invention are:
(1) according to the method, a micro negative pressure environment is created at a gas-liquid interface above the silicon melt in the external refining process of the industrial silicon furnace, so that volatile impurities in the silicon melt are efficiently removed in the external refining process of the silicon melt, and harmful substances such as smoke, dust and the like generated in the external refining process are exhausted through a micro negative pressure vacuum device after absorption treatment, so that efficient impurity removal and clean production in the external refining process of the silicon melt are realized;
(2) the method can greatly reduce or avoid the use of industrial oxygen, air and slag former in the conventional external refining process of the industrial silicon melt, reduces the emission of industrial three wastes such as silicon oxide smoke dust, silicon smelting slag and the like in the production process, has economic advantages, and meets the requirements of environmental protection.
(3) Aiming at the existing industrial silicon melt external refining technology, the method of the invention does not need to modify and upgrade the existing equipment, also reduces the special requirements on the erosion resistance, the strength and the like of the furnace lining material of the external refining equipment in the conventional process, and has the advantages of simple equipment, easy operation, suitability for large-scale industrial production and the like.
Drawings
FIG. 1 is a schematic view of a micro-negative pressure device and an external refining device;
fig. 2 is a schematic view of the elevation-rotation member connection.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but the scope of the present invention is not limited to the description.
The invention relates to a schematic diagram of a micro negative pressure device and an external refining device, which is shown in figure 1, wherein the micro negative pressure device comprises a smoke collecting hood, a flue, a vacuum unit and a dust collecting device which are sequentially connected, the smoke collecting hood is arranged right above a ladle port of the external refining device, and the smoke collecting hood is hermetically connected with the ladle port of the external refining device to form a closed cavity; the outer wall of the smoke collecting hood can be suspended by a crown block or is connected with a lifting-rotating component system, the lifting-rotating component comprises a controller, a driving servo motor I and a driving servo motor II, the device comprises a transmission shaft I, a transmission shaft II and a clamping connecting rod, wherein one end of the clamping connecting rod is fixedly connected with the outer wall of the smoke collecting hood, the other end of the clamping connecting rod is fixedly connected with the top end of the transmission shaft I, the bottom end of the transmission shaft I is connected with the top end of the transmission shaft II through a ball bearing or a needle bearing, the transmission shaft I can rotate at the top end of the transmission shaft II, the bottom end of the transmission shaft II is fixedly connected with an output shaft of a driving servo motor II, the driving servo motor II is a stepping reciprocating motor, the driving servo motor I is fixedly arranged on the transmission shaft II through a supporting rod, a gear I is arranged on the output shaft of the driving servo motor I, a gear II is sleeved on the transmission shaft I, and the gear I and the gear II are positioned on the same horizontal plane and are in meshed transmission; the driving servo motor I and the driving servo motor II are respectively and electrically connected with a controller (see figure 2); the outer wall of the smoke collecting hood is provided with a fire-resistant layer and a cooling water jacket; the top opening of the external refining device can be used for introducing gas from the top, adding a slagging agent and pouring slag and silicon liquid, smoke and dust fume generated in the refining process is generated at a gas-liquid interface and collected in a fume collecting hood under the action of micro negative pressure, the area of a fume collecting hood opening can cover the whole top opening of the external refining device, and a lifting-rotating member of the fume collecting hood can be adjusted in height according to different refining periods, for example, the fume collecting hood can be properly lifted in the ventilation process and the slagging agent adding process, and the fume collecting hood can be lifted to a specific height in the silicon liquid adding or discharging process; the fire-resistant layer of the smoke collecting hood can ensure that the smoke collecting hood can bear different refining temperatures; the smoke collecting hood can be in the shape of a round bottom, a conical shape, a tetrahedral frustum and the like, and the specific size and the cross section shape can be determined according to the geometrical shape and the size of a top opening of a specific external refining device so as to ensure the complete connection between the smoke collecting hood and a furnace opening, thereby avoiding the escape, the overflow, the leakage and the like of furnace gas and ensuring the micro negative pressure environment in the smoke collecting hood; the smoke collecting hood can be made of a stainless steel shell layer, a steel sleeve and the like, and the outer wall of the smoke collecting hood is lined with a fire-resistant layer and a cooling water jacket, so that the rigidity, the strength and the high temperature resistance of the smoke collecting hood are ensured, and the pollution of an external pollution source to the silicon melt is avoided; the vacuum equipment of the vacuum device is a one-stage or multi-stage combined vacuum pump, and the vacuum pump is a rough pumping mechanical pump or a molecular pump; the vacuum system can be determined according to the content and the type of impurities in silicon melts from different sources or in different batches, for example, the silicon melt containing higher volatile impurities can adopt a multi-stage vacuum pump to keep the furnace mouth at a relatively higher vacuum degree, so that the deep removal of a large amount of volatile impurities is ensured, and the refining period can be effectively shortened; the dust collecting system can be a cloth bag, cyclone, gravity or electrostatic dust collecting equipment and can simultaneously collect micro silicon powder, silicon powder and the like carried in smoke dust in the refining process outside the furnace.
Example 1: a micro-negative pressure external refining method of industrial silicon melt comprises the following specific steps:
(1) in the production of certain industrial silicon smelting enterprises in Yunnan, about 2 tons of silicon melt discharged from a submerged arc ore thermoelectric furnace is contained in an external refining ladle, and in order to further reduce Al and Ca, the silicon melt in the ladle is subjected to oxidation blowing refining again; the impurity content in the silicon melt is 8000ppm and 15000ppm in terms of mass percent;
(2) oxidizing and blowing refining the silicon melt obtained in the step (1), wherein the blowing mode of the oxidizing and blowing refining is top blowing ventilation, the gas is industrial oxygen, the top blowing ventilation time is 0.5h, the top blowing ventilation pressure is 1.2-2 atmospheric pressures, and the gas flow rate is 0.2-1 m 3 /s；
(3) Carrying out micro negative pressure external refining while carrying out oxidation blowing refining in the step (2), moving a smoke collecting hood of a micro negative pressure device to be right above a ladle opening of the external refining device through a lifting-rotating component, enabling the smoke collecting hood opening to cover the ladle opening, starting a vacuum device (a two-stage combined mechanical vacuum pump) of the micro negative pressure device to carry out micro negative pressure external refining on the industrial silicon melt, wherein the pressure of the ladle opening is about 0.1 atmosphere, and the time of the micro negative pressure external refining lasts for 5-10min after ventilation is finished so as to remove volatile impurities in the industrial silicon melt;
(4) Closing the micro negative pressure external refining device after the micro negative pressure external refining is finished, moving the micro negative pressure external refining device to an initial position, and carrying out external casting on the impurity-removed silicon melt refined by the micro negative pressure external refining in the step (3) to obtain an impurity-removed industrial silicon product;
in percentage by mass, the impurity content in the impurity-removed industrial silicon product is less than 2000ppm of Al and less than 1000ppm of Ca.
Example 2: a micro-negative pressure external refining method of industrial silicon melt comprises the following specific steps:
(1) in the production of certain industrial silicon smelting enterprises in Yunnan, about 2 tons of silicon melt discharged from a submerged arc ore thermoelectric furnace is contained in a refining ladle outside the furnace, and in order to further reduce Al and Ca, the silicon melt in the ladle is subjected to slagging refining; in percentage by mass, the impurity content in the silicon melt is 6000ppm of Al and 1300ppm of Ca;
(2) adding a slagging agent CaO into the silicon melt in the step (1), and then introducing industrial compressed nitrogen for slagging refining, wherein the adding amount of the slagging agent CaO is 2 kg/ton and the introducing time of the industrial compressed nitrogen is 15min based on the silicon melt;
(3) carrying out micro-negative pressure external refining while carrying out slagging refining in the step (2), moving a smoke collecting hood of a micro-negative pressure device to be right above a ladle opening of the external refining device through a lifting-rotating component so that the smoke collecting hood opening can cover the ladle opening, and starting a vacuum device (a two-stage combined mechanical vacuum pump) of the micro-negative pressure device so as to carry out micro-negative pressure external refining on the industrial silicon melt, wherein the pressure of the ladle opening is about 0.1 atmosphere, and the time of the micro-negative pressure external refining lasts for 5-10min after ventilation is finished so as to remove volatile impurities in the industrial silicon melt;
(4) Closing the micro negative pressure external refining device after the micro negative pressure external refining is finished, moving the micro negative pressure external refining device to an initial position, and carrying out external casting on the impurity-removed silicon melt refined by the micro negative pressure external refining in the step (3) to obtain an impurity-removed industrial silicon product;
in percentage by mass, the impurity content in the impurity-removed industrial silicon product is Al <1200ppm and Ca <800 ppm.
Example 3: a micro-negative pressure external refining method of industrial silicon melt comprises the following specific steps:
(1) in the production of certain industrial silicon smelting enterprises in Yunnan, about 2 tons of silicon melt discharged from a submerged arc ore thermoelectric furnace is contained in a refining ladle outside the furnace, and in order to further reduce Al and Ca, the silicon melt in the ladle is subjected to blowing-slagging composite refining; the impurity content of the silicon melt is 5000ppm of Al and 1100ppm of Ca in percentage by mass;
(2) adding a slagging agent CaO into the silicon melt in the step (1), and then introducing industrial oxygen for blowing-slagging composite refining, wherein the adding amount of the slagging agent CaO is 1 kg/ton based on the silicon melt, the introduction mode of the industrial oxygen is top blowing, the aeration time of the industrial oxygen is 10min, the aeration pressure is 1.2-2 atmospheric pressures, and the gas flow rate is 0.2-1m 3 /s；
(3) Carrying out micro-negative pressure external refining while carrying out slagging refining in the step (2), moving a smoke collecting hood of a micro-negative pressure device to be right above a ladle opening of the external refining device through a lifting-rotating component so that the smoke collecting hood opening can cover the ladle opening, and starting a vacuum device (a two-stage combined mechanical vacuum pump) of the micro-negative pressure device so as to carry out micro-negative pressure external refining on the industrial silicon melt, wherein the pressure of the ladle opening is about 0.1 atmosphere, and the time of the micro-negative pressure external refining lasts for 5-10min after ventilation is finished so as to remove volatile impurities in the industrial silicon melt;
(4) closing the micro negative pressure external refining device after the micro negative pressure external refining is finished, moving the micro negative pressure external refining device to an initial position, and carrying out external casting on the impurity-removed silicon melt refined by the micro negative pressure external refining in the step (3) to obtain an impurity-removed industrial silicon product;
in percentage by mass, the impurity content in the impurity-removed industrial silicon product is Al <600ppm and Ca <800 ppm.
Claims (2)
1. A micro-negative pressure external refining method of industrial silicon melt is characterized by comprising the following specific steps:
moving the micro negative pressure device to be right above a ladle opening of the external refining device, and starting a vacuum device of the micro negative pressure device to carry out micro negative pressure external refining on the industrial silicon melt so as to remove volatile impurities in the industrial silicon melt;
The micro negative pressure device comprises a smoke collecting hood, a flue, a vacuum unit and a dust collecting device which are sequentially connected, wherein the smoke collecting hood is arranged right above a ladle port of the external refining device, and the smoke collecting hood is hermetically connected with the ladle port of the external refining device to form a closed cavity; the smoke collecting hood is hermetically connected with the ladle opening of the external refining device to form a closed cavity; the outer wall of the smoke collecting hood is connected with a crown block suspension or lifting-rotating component system.
2. A process for silicon melt micro negative pressure external refining as set forth in claim 1 wherein: the external refining comprises blowing refining, slagging refining or blowing-slagging composite refining.
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