CN219009925U - High-efficient environment-friendly arsenic trichloride preparation facilities - Google Patents
High-efficient environment-friendly arsenic trichloride preparation facilities Download PDFInfo
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- CN219009925U CN219009925U CN202222800616.XU CN202222800616U CN219009925U CN 219009925 U CN219009925 U CN 219009925U CN 202222800616 U CN202222800616 U CN 202222800616U CN 219009925 U CN219009925 U CN 219009925U
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Abstract
The utility model relates to a high-efficiency environment-friendly arsenic trichloride preparation device, which comprises a furnace body; a closed furnace chamber is formed in the furnace body; the furnace chamber is a preparation area in the area close to the middle and is used for carrying out the preparation operation of arsenic trichloride; the furnace chamber is provided with a dechlorination area at the lower part of the preparation area and is used for dechlorination and purification operation, and the bottom side area of the furnace chamber is provided with a collection area and is used for collecting liquid arsenic trichloride; the furnace body is also provided with a chlorine gas supply assembly, and the gas outlet end of the chlorine gas supply assembly is positioned in the preparation area; a pore plate is also arranged in the dechlorination zone and is used for bearing raw material arsenic; the pore plate is provided with a plurality of small holes for the liquid arsenic trichloride to pass through. The high-efficiency environment-friendly arsenic trichloride preparation device can improve the preparation efficiency of arsenic trichloride, reduce the labor intensity and effectively reduce the content of free chlorine in the arsenic trichloride; the preparation process is in a relatively sealed environment, so that the emission of toxic and harmful gases can be effectively reduced, and the environmental protection requirement in the process of preparing the arsenic trichloride is met.
Description
Technical Field
The utility model relates to the field of arsenic trichloride production equipment, in particular to a high-efficiency environment-friendly arsenic trichloride preparation device.
Background
Arsenic trichloride is an inorganic compound with a chemical formula of AsCl 3 The melting point is low, and the liquid is liquid at normal temperature, so that the liquid is colorless or light yellow fuming liquid. Arsenic trichloride is toxic and highly corrosive. Dissolving in ethanol, diethyl ether and concentrated hydrochloric acid at normal temperature, decomposing in water and ultraviolet, and giving off white smoke-like irritant and corrosive hydrogen chloride gas. Mixing with sodium, potassium and aluminum, and can be exploded violently after impact. Arsenic trichloride is exposed to air and hydrolyzed to arsenite and hydrogen chloride, and white smoke is generated. Is soluble in water and plays a role in hydrolysis. Decomposing in water to generate arsenic hydroxide and hydrogen chloride, and fuming in air.
The high-purity arsenic trichloride can be used as a semiconductor material and a raw material for synthesizing an arsenic-containing organic compound, and can also be used as a raw material for preparing high-purity arsenic or used in the field of pesticides and the like. With the development of semiconductor material technology, the demand for high-purity arsenic has been increasing year by year, so the demand for raw material arsenic trichloride for producing high-purity arsenic has also been increasing.
At present, two main methods for preparing arsenic trichloride are available, one is prepared by reacting concentrated hydrochloric acid with arsenic trioxide; the other is prepared by directly reacting metal arsenic with chlorine. Arsenic trioxide, commonly known as "arsenic," has strong toxicity. When arsenic trioxide and hydrochloric acid are adopted to react to prepare arsenic trichloride, the danger is high, and meanwhile, certain influence is caused on the environment, and the preparation mode is generally not adopted in the conventional preparation process. The method for preparing the arsenic trichloride in the industry mainly adopts the direct reaction of metal arsenic and chlorine, wherein the reaction of the arsenic and the chlorine is exothermic, and a large amount of heat is generated in the process; and excessive chlorine is needed during the reaction, so that the free chlorine content in the prepared arsenic trichloride is higher. At present, a device for preparing arsenic trichloride by adopting the reaction of chlorine and arsenic in the industry mainly uses quartz equipment, so that the single furnace feeding amount is low, the feeding times are frequent, and the labor intensity is high; meanwhile, the equipment is semi-sealed, toxic and harmful gases generated in the process are directly pumped away by an external fan, and the production condition is bad, so that the equipment has a certain influence on the environment.
Therefore, a high-efficiency environment-friendly arsenic trichloride preparation device needs to be studied to meet the requirement of raw materials in the preparation process of high-purity arsenic, and meanwhile, the development requirement of the semiconductor industry is met. And related equipment for preparing the efficient and environment-friendly arsenic trichloride is not available in the current searched data. Therefore, the development of the high-efficiency environment-friendly arsenic trichloride preparation device can meet the requirements of preparing high-purity arsenic and reduce the pollution to the environment in the process.
Disclosure of Invention
In order to solve the technical problems, the utility model provides the efficient and environment-friendly arsenic trichloride preparation device, which can improve the preparation efficiency of arsenic trichloride, reduce the labor intensity and reduce the content of free chlorine in the prepared arsenic trichloride; meanwhile, the device is in a relatively sealed environment during operation, so that the emission of toxic and harmful gases in the preparation process can be effectively reduced; meets the requirements of the high-purity arsenic preparation industry on raw material arsenic trichloride and the environmental protection requirement in the process of preparing the arsenic trichloride.
The technical scheme adopted for solving the technical problems is as follows: an efficient and environment-friendly arsenic trichloride preparation device comprises a furnace body; a closed furnace chamber is formed in the furnace body; the furnace chamber is a preparation area in the area close to the middle and is used for carrying out the preparation operation of arsenic trichloride in the area; the furnace chamber is provided with a dechlorination area at the lower part of the preparation area and is used for dechlorination and purification in the area, and the bottom side area of the furnace chamber is provided with a collecting area and is used for collecting liquid arsenic trichloride in the area; the furnace body is also provided with a chlorine gas supply assembly, and the gas outlet end of the chlorine gas supply assembly is positioned in the preparation area; a pore plate is also arranged in the dechlorination zone and is used for bearing raw material arsenic; the pore plate is provided with a plurality of small holes for the liquid arsenic trichloride to pass through.
Further, the outer side of the furnace body is provided with a cooling assembly and a first temperature sensor at a position corresponding to the preparation area, and the working end of the first temperature sensor is positioned in the preparation area; the cooling component is matched with the first temperature sensor and used for adjusting the temperature of the preparation area; the outside of furnace body still is provided with heating element and second temperature sensor in the position that corresponds with the dechlorination district, and heating element cooperates with second temperature sensor for adjust the temperature in dechlorination district.
Further, a discharging pipeline assembly is arranged at the bottom side of the collecting area and used for discharging liquid arsenic trichloride; a discharge control valve is arranged on a pipeline of the discharge pipeline assembly; the bottom of the collecting area is also provided with a deslagging pipeline assembly for deslagging, and a deslagging control valve is arranged on a pipeline of the deslagging pipeline assembly.
Further, a first gas pipeline assembly is arranged at the upper position of the furnace body, and the gas inlet end of the first gas pipeline assembly is communicated with the furnace chamber of the furnace body; an exhaust valve is arranged on a pipeline of the first gas pipeline assembly; a safety valve is arranged between the furnace body and the exhaust valve on the pipeline of the first gas pipeline assembly; the first gas pipeline component is used for regulating the pressure of the furnace chamber and discharging tail gas; the upper position of the furnace body is also provided with a pressure sensor for monitoring the pressure of the furnace chamber.
Further, an arsenic feeding assembly is arranged above the furnace body, and the discharge end of the arsenic feeding assembly is communicated with the furnace chamber; the arsenic charging assembly comprises an arsenic charging cavity, an arsenic discharging pipe is arranged at the bottom side of the arsenic charging cavity and used as a discharging end of the arsenic charging assembly, and an arsenic charging control valve is arranged between the arsenic discharging pipe and the furnace chamber; the top side of the arsenic charging cavity of the arsenic charging assembly is also provided with a charging cover plate for opening or closing a charging opening of the arsenic charging cavity; the charging cover plate is locked with the arsenic charging cavity through a quick connecting piece.
Further, a second gas pipeline assembly is arranged on the arsenic charging assembly; an air inlet valve is arranged on a pipeline of the second gas pipeline assembly; the second gas pipeline component is used for introducing protective gas into the arsenic charging cavity and the furnace chamber.
Further, the chlorine gas supply assembly comprises a chlorine gas supply main pipe, a section of the chlorine gas supply main pipe, which is positioned outside the furnace body, is provided with a chlorine gas regulating valve and a chlorine gas flowmeter, and the tail end of the section of the chlorine gas supply main pipe, which is positioned in the furnace chamber, extends to the preparation area; the tail end of the chlorine gas supply main pipe is communicated with a plurality of chlorine gas supply branch pipes; the chlorine gas supply branch pipe is radially arranged by taking the tail end of the chlorine gas main pipe as the center; the chlorine gas supply branch pipes are uniformly distributed in a circle taking the tail end of the chlorine gas main pipe as the center; the chlorine gas supply branch pipe is positioned at a position close to the bottom side in the preparation area; one end of the chlorine gas supply branch pipe, which is far away from the tail end of the chlorine gas main pipe, is bent upwards towards the center to form an air outlet nozzle; the air outlet of the air outlet nozzle is not upward.
Further, the arsenic trichloride preparation device also comprises a control module, wherein the control module is in communication connection with the air inlet valve, the air outlet valve, the pressure sensor, the arsenic feeding control valve, the chlorine regulating valve, the chlorine flowmeter, the cooling assembly, the first temperature sensor, the heating assembly and the second temperature sensor.
Further, a furnace cover is arranged on the top side of the furnace body, and the furnace cover is fixed with the furnace body through a fastener; the arsenic charging assembly is arranged on the furnace cover.
Furthermore, the furnace body is also provided with an observation mirror at the position of the preparation area, and a cooling mechanism is arranged at the position of the observation mirror.
The utility model has the advantages that: according to the high-efficiency environment-friendly arsenic trichloride preparation device, arsenic trichloride preparation and arsenic trichloride dechlorination are integrated into one furnace body, so that the free chlorine content in arsenic trichloride generated by the reaction of excessive chlorine and arsenic can be effectively reduced, the utilization rate of chlorine elements is improved, the condition that chloride ions in a downstream arsenic trichloride purification process enter the environment is avoided, the problem that a separate dechlorination device is matched for dechlorination treatment in conventional production is solved, and the production efficiency is improved; the cooling component arranged in the preparation area can effectively regulate the heat generated during the preparation of arsenic trichloride; the heating component arranged in the dechlorination area can control the temperature of the dechlorination area, so that the requirement of improving the dechlorination effect is met; the arsenic feeding assembly is designed, the single feeding amount is large, an independent sealed feeding system is adopted in the feeding process, the arsenic feeding control valve is adjusted to feed the arsenic, and inert gas is introduced into the arsenic feeding assembly through the second gas pipeline assembly to protect the arsenic feeding assembly in the feeding process, so that toxic and harmful gas in the furnace body cannot escape into the environment; the chlorine gas inlet device is designed, and a plurality of chlorine gas inlet branch pipes are adopted for simultaneously inlet gas, so that raw material arsenic and chlorine gas in the furnace body react at a plurality of point positions, the contact area is large, and the reaction efficiency is high; the monitoring data of each sensor is received through the control module, and the opening or closing of each valve is controlled according to the monitoring data, so that the automatic control degree is high, the labor intensity is low, the production efficiency is high, and the safety is good.
Drawings
FIG. 1 is a schematic diagram of an efficient and environment-friendly arsenic trichloride production apparatus according to a first embodiment;
FIG. 2 is a schematic perspective view showing the distribution of chlorine gas supply branch pipes of a high-efficiency environment-friendly arsenic trichloride production apparatus according to the first embodiment;
the furnace comprises a 1-furnace body, a 2-chlorine gas supply assembly, a 3-first gas pipeline assembly, a 4-arsenic charging assembly, a 5-second gas pipeline assembly, a 6-pressure sensor, a 11-preparation area, a 12-dechlorination area, a 13-collection area, a 14-discharge pipeline assembly, a 15-slag discharge pipeline assembly, a 16-furnace cover, a 17-observation mirror, a 21-chlorine gas supply main pipe, a 22-chlorine gas supply branch pipe, a 23-air outlet nozzle, a 24-chlorine gas regulating valve, a 25-chlorine gas flowmeter, a 31-safety valve, a 32-exhaust valve, a 41-arsenic charging cavity, a 42-arsenic discharging pipe, a 43-arsenic charging control valve, a 44-charging cover plate, a 51-inlet valve, a 111-cooling assembly, a 112-first temperature sensor, a 121-pore plate, a 122-heating assembly, a 123-second temperature sensor, a 141-discharge control valve, a 151-slag discharge control valve, 161-fastening piece, a 171-mirror cooling water inlet channel, a 172-mirror cooling water outlet channel, a 441-quick connector, a 1111-cooling assembly inlet valve, a 1112-cooling assembly water outlet valve.
Detailed Description
The present utility model will be further described in detail with reference to the drawings and examples, which are only for the purpose of illustrating the utility model and are not to be construed as limiting the scope of the utility model.
Example 1
Referring to fig. 1 and 2, the embodiment provides a high-efficiency environment-friendly arsenic trichloride preparation device, which comprises a furnace body 1; a closed furnace chamber is formed in the furnace body 1; the furnace chamber is provided with a preparation area 11 near the middle for carrying out the preparation operation of arsenic trichloride in the area; the furnace chamber is provided with a dechlorination zone 12 in the lower area of the preparation zone 11 for dechlorination and purification operation in the area, and a collection zone 13 in the bottom side area of the furnace chamber for collecting liquid arsenic trichloride in the area; the furnace body 1 is also provided with a chlorine gas supply assembly 2, and the gas outlet end of the chlorine gas supply assembly 2 is positioned in a preparation area 11; a pore plate 121 is also arranged in the dechlorination zone 12 and is used for bearing raw material arsenic; the orifice plate 121 is provided with a plurality of small holes for the passage of liquid arsenic trichloride.
In this embodiment, when the orifice plate 121 is used, the raw arsenic in the form of a block is deposited as dechlorination filler for free chlorine in arsenic trichloride; stacking raw material arsenic for synthesizing arsenic trichloride on the blocky raw material arsenic; a plurality of small holes are distributed on the pore plate, the diameter of the small holes is 3-5mm, and the interval between the holes is 2-4mm; the raw material arsenic can be well blocked by the holes, and liquid arsenic trichloride generated by the reaction can pass through the holes and enter the collecting area.
Referring to fig. 1 again, the outside of the furnace body 1 is provided with a cooling assembly 111 and a first temperature sensor 112 at a position corresponding to the preparation area 11, and the working end of the first temperature sensor 112 is located in the preparation area 11; the cooling assembly 111 cooperates with a first temperature sensor 112 for regulating the temperature of the preparation zone 11. In this embodiment, the cooling component may adopt a jacket type cooling water cooling mechanism, the water inlet end of the cooling component 111 is provided with a cooling component water inlet valve 1111 and a cooling component water outlet valve 1112, the water inlet rate of the cooling water is adjusted by the cooling component water inlet valve, so as to timely take away the heat generated by the reaction of chlorine and arsenic in the preparation area, the first temperature sensor 112 may be a thermocouple, and the cooling component water inlet valve 1111 and the thermocouple form a linkage signal feedback, so that the temperature of the preparation area is stably controlled in a required temperature interval.
Referring to fig. 1 again, a heating assembly 122 and a second temperature sensor 123 are further disposed on the outer side of the furnace body 1 at a position corresponding to the dechlorination zone 12, and the heating assembly 122 is matched with the second temperature sensor 123 to adjust the temperature of the dechlorination zone 12. In this embodiment, the heating component 122 is used to heat the blocky raw material arsenic as dechlorinated packing on the pore plate, so as to improve dechlorination effect, and the heating component 122 can use a resistance heating furnace; the second temperature sensor 123 may be a temperature control thermocouple; the working end of the temperature control couple is close to the furnace wall; the dechlorination effect can be effectively improved by heating the dechlorination area and precisely controlling the temperature.
Referring again to fig. 1, a discharging pipeline assembly 14 is arranged at the bottom side of the collecting area 13, and is used for discharging liquid arsenic trichloride; a discharge control valve 141 is arranged on a pipeline of the discharge pipeline assembly 14; the bottommost part of the collecting area is also provided with a deslagging pipeline assembly 15 for deslagging, and a deslagging control valve 151 is arranged on a pipeline of the deslagging pipeline assembly 15. In the implementation, the output end of the discharging pipeline component can be connected with an arsenic trichloride storage tank; the output end of the slag discharging pipeline component is connected with the residue treatment system.
Referring to fig. 1 again, the furnace body 1 is further provided with a first gas pipeline assembly 3 at an upper position, and an air inlet end of the first gas pipeline assembly 3 is communicated with a furnace chamber of the furnace body 1; an exhaust valve 32 is arranged on the pipeline of the first gas pipeline assembly 3; a safety valve 31 is arranged between the furnace body 1 and the exhaust valve 32 on the pipeline of the first gas pipeline assembly 3; the first gas pipeline assembly 3 is used for regulating the pressure of the furnace chamber and discharging tail gas; the furnace body 1 is also provided with a pressure sensor 6 at an upper position for monitoring the pressure of the furnace chamber.
Referring to fig. 1 again, an arsenic charging assembly 4 is further arranged above the furnace body 1, and a discharging end of the arsenic charging assembly 4 is communicated with the furnace chamber; the arsenic charging assembly 4 comprises an arsenic charging cavity 41, an arsenic discharging pipe 42 is arranged at the bottom side of the arsenic charging cavity 41 and used as a discharging end of the arsenic charging assembly 4, and an arsenic charging control valve 43 is arranged between the arsenic discharging pipe 42 and the furnace chamber; the top side of the arsenic charging cavity 41 of the arsenic charging assembly 4 is also provided with a charging cover plate 44 for opening or closing a charging opening of the arsenic charging cavity 41; the feed cap 44 is locked to the arsenic feed cavity 41 by a quick connector 441. In the embodiment, the charging cover plate can be used for rapidly opening or closing a charging opening of the arsenic charging cavity, and particularly, the charging cover plate and the arsenic charging cavity are fastened through a rapid connecting buckle, and the charging cover plate and the arsenic charging cavity are sealed through a sealing piece; during charging, an arsenic charging control valve is used for controlling; during preparation, the arsenic feeding control valve is in a closed state.
Referring again to fig. 1, the arsenic charging assembly 4 is provided with a second gas line assembly 5; an air inlet valve 51 is arranged on a pipeline of the second air pipeline assembly 5; the second gas pipeline assembly 5 is used for introducing protective gas into the arsenic-charging cavity 41 and the furnace chamber. In this embodiment, the second gas pipeline assembly 5 is preferably used for providing inert gas; during charging, an air inlet valve is required to be opened, and inert gas (such as argon) is introduced, so that the charging cavity is in positive pressure relative to the furnace chamber, and toxic and harmful gas in the furnace chamber is prevented from escaping.
Referring to fig. 1 and 2 again, the chlorine gas supply assembly 2 comprises a chlorine gas supply main pipe 21, a section of the chlorine gas supply main pipe 21, which is positioned outside the furnace body, is provided with a chlorine gas regulating valve 24 and a chlorine gas flowmeter 25, and the tail end of the section of the chlorine gas supply main pipe, which is positioned in the furnace chamber, extends to the preparation area; the tail end of the chlorine gas supply main pipe 21 is communicated with a plurality of chlorine gas supply branch pipes 22; the chlorine gas supply branch pipe 22 is radially arranged with the tail end of the chlorine gas main pipe 21 as the center; the chlorine gas supply branch pipes 22 are uniformly distributed in a circle centering on the end of the chlorine gas main pipe 21; the chlorine gas supply branch pipe 22 is positioned near the bottom side in the preparation area; the chlorine gas supply branch pipe 22 is bent upwards to the center at one end far away from the tail end of the chlorine gas main pipe 21 to form an air outlet nozzle 23; the outlet of the outlet nozzle 23 is not upward. In the embodiment, the chlorine gas supply main pipe is generally positioned in the axial center area of the furnace body, four chlorine gas supply branch pipes 22 are adopted, the included angle between two adjacent chlorine gas supply branch pipes is 90 degrees, and when the arsenic trichloride is prepared, chlorine gas can be simultaneously supplied from four directions so as to improve the reaction efficiency of the arsenic and the chlorine gas; meanwhile, due to the inclined arrangement of the air outlet nozzle and the air outlet, raw material arsenic falls into the air outlet to block the air outlet during charging, and in addition, the design of the air outlet nozzle is beneficial to increasing the contact area between chlorine and arsenic so as to achieve better chlorination efficiency.
In this embodiment, the arsenic trichloride production apparatus further includes a control module, which is communicatively connected to the air intake valve 51, the air exhaust valve 32, the pressure sensor 6, the arsenic feed control valve 43, the chlorine regulating valve 24, the chlorine flow meter 25, the cooling module 111, the first temperature sensor 112, the heating module 122, and the second temperature sensor 123. In this embodiment, the arsenic charging control valve, the air inlet valve and the air outlet valve are all valves capable of being opened and closed in response to the control command of the control module; the control module receives pressure data in the furnace chamber of the pressure sensor, and controls the exhaust valve to be opened when the pressure value reaches a set value; the air inflow of the chlorine is monitored through a chlorine flow meter and controlled through a chlorine air inflow regulating valve, the air inflow of the chlorine can be properly controlled according to the temperature of a preparation area in a furnace chamber, a control module receives temperature data of the preparation area of a first temperature sensor, and after the temperature exceeds a set value, the chlorine air inflow regulating valve is controlled to control the air inflow of the chlorine; the safety valve and the pressure sensor form interlocking control, when the pressure in the furnace body exceeds a maximum set value, the safety valve is tripped and opened, and pressure relief treatment is carried out to protect the safe operation of the furnace body; the control module receives temperature data detected by the first temperature sensor, and controls the heating assembly to heat according to the set temperature parameters, so that accurate temperature control is realized.
Referring to fig. 1 again, a furnace cover 16 is arranged on the top side of the furnace body 1, and the furnace cover 16 is fixed with the furnace body 1 through a fastener 161; the arsenic charging assembly 4 is mounted on a furnace lid 16. In this embodiment, the fastener 161 may be a fastening bolt, and the furnace cover is fixed on the furnace body by the fastening bolt, and the furnace body and the furnace cover are sealed by a sealing member; the design of bell for the device is when overhauing, conveniently dismantles the bell, provides the access hole.
Referring again to fig. 1, the furnace body 1 is further provided with an observation mirror 17 at the position corresponding to the preparation area 11, and a cooling mechanism is arranged at the position of the observation mirror 17. In this embodiment, the reaction condition of arsenic and chlorine and the consumption condition of raw material arsenic can be observed through the observation mirror 17, the observation mirror is made of two layers of pressure-resistant thickened quartz, a jacket cooling water cooling structure is arranged in the middle, and a mirror cooling water inlet channel 171 and a mirror cooling water outlet channel 172 are arranged.
Example two
The embodiment provides a method for preparing arsenic trichloride by using a high-efficiency environment-friendly arsenic trichloride preparation device, which comprises the following steps:
s1, washing the surfaces of raw material industrial arsenic ingots with purity of 99% by pure water, airing and crushing the raw material industrial arsenic ingots into crushed blocks with the size of less than 50mm for later use;
s2, opening an arsenic charging control valve, opening an air inlet valve of a second gas pipeline assembly on the arsenic charging assembly and an air outlet valve of a first gas pipeline assembly on the furnace body, continuously introducing argon for 15min to replace air in the furnace chamber, weighing 20kg of the block raw material arsenic (without powder) prepared in the step S1, adding the block raw material arsenic into a pore plate of the furnace chamber through the arsenic charging assembly, and finally weighing 80kg of raw material arsenic into the device;
s3, after the charging is completed, sequentially closing an air inlet valve, an arsenic charging control valve and an air outlet valve, covering a charging cover plate of the arsenic charging assembly, and fixing the charging cover plate at a charging port of an arsenic charging cavity by a compression quick connecting piece;
s4, starting a heating assembly, heating to 80-120 ℃ according to a set temperature, and maintaining the temperature;
s5, opening a cooling component water inlet valve of the cooling component and a sight glass cooling water inlet channel; the chlorine regulating valve is opened, the flow rate of the chlorine is controlled to be 800-1200L/h, at the moment, the reaction condition in the furnace can be checked from an observation mirror on the furnace body, meanwhile, the temperature of the preparation area is set to be 100-150 ℃, once the monitored temperature value of the first temperature sensor exceeds a set value, the control module controls the chlorine regulating valve and the water inlet valve of the cooling assembly, and the flow rates of the chlorine and the cooling water are regulated;
s6, free chlorine generated by excessive chlorine is removed when arsenic trichloride formed after the reaction of chlorine and arsenic is subjected to a dechlorination device, and the free chlorine is subjected to a dechlorination filler formed by blocky arsenic and then is reacted at the temperature of 80-120 ℃ to produce arsenic trichloride, so that the free chlorine in the arsenic trichloride is removed;
s7, after chlorine is introduced to react for about 2 hours, a discharge control valve at the bottom of the furnace body is opened, and the synthesized arsenic trichloride is sent to an arsenic trichloride storage tank;
s8, checking the reaction condition of the preparation area through an observation mirror at any time in the preparation process, once the height of the raw material arsenic for reaction is lower than that of an air outlet nozzle of the chlorine air supply assembly, immediately closing a chlorine regulating valve, and opening an air outlet valve and an air inlet valve and then carrying out the charging operation of a second furnace;
and S9, after continuously running for 5-8 times, opening a slag discharging control valve of a slag discharging pipeline assembly at the bottom of the furnace body to perform slag discharging once, and collecting discharged waste slag intensively to be used as a raw material for preparing arsenic trichloride.
In the embodiment, the preparation process is always carried out in a closed environment, and the generated tail gas enters a tail gas treatment system without harmful gas leakage; 80kg of arsenic is fed, the reaction period is 12-15 hours, the efficiency is high, the operation is simple, and the labor intensity is low.
Comparative example one
The present comparative example differs from the first example in that: in the step S2, the argon valve is closed, and only the tail gas valve is opened; there is no dechlorination device using blocky arsenic as filler in the step S6. The other is the same as in the first embodiment.
In the comparative example, during the operation of charging, the environment has pungent smell, which can cause harm to operators and pollute the environment; the prepared arsenic trichloride contains a large amount of free chlorine, and a separate arsenic trichloride dechlorination device is required to dechlorinate in the arsenic trichloride purification process.
Comparative example two
The present comparative example differs from the first example in that: in step S5, the chlorine gas inlet pipeline is an air inlet nozzle of a conventional quartz synthesizer, and no cooling component and temperature regulation control of a preparation area are provided. The other is the same as in the first embodiment.
In the comparative example, the reaction of chlorine and arsenic is exothermic, excessive chlorine is needed in the process, an operator manually adjusts the air inflow of the chlorine according to experience, the temperature of a preparation device is high, excessive chlorine in a furnace leads to excessive pressure, a safety valve frequently jumps to carry out pressure relief protection in the furnace, the utilization rate of the chlorine is low, and the chlorine is lost through tail gas; 80kg of arsenic is fed, the reaction period is 40-45 hours, and the production efficiency is low.
The above embodiments should not limit the present utility model in any way, and all technical solutions obtained by equivalent substitution or equivalent conversion fall within the protection scope of the present utility model.
Claims (10)
1. An efficient environment-friendly arsenic trichloride preparation device is characterized in that: comprises a furnace body; a closed furnace chamber is formed in the furnace body; the furnace chamber is a preparation area in the area close to the middle and is used for carrying out the preparation operation of arsenic trichloride; the furnace chamber is provided with a dechlorination area at the lower part of the preparation area and is used for dechlorination and purification operation, and the bottom side area of the furnace chamber is provided with a collection area and is used for collecting liquid arsenic trichloride; the furnace body is also provided with a chlorine gas supply assembly, and the gas outlet end of the chlorine gas supply assembly is positioned in the preparation area; a pore plate is also arranged in the dechlorination zone and is used for bearing raw material arsenic; the pore plate is provided with a plurality of small holes for the liquid arsenic trichloride to pass through.
2. The efficient and environment-friendly arsenic trichloride preparation device as claimed in claim 1, wherein: the outer side of the furnace body is arranged at a position corresponding to the preparation area, and is also provided with a cooling assembly and a first temperature sensor, and the working end of the first temperature sensor is positioned in the preparation area; the cooling component is matched with the first temperature sensor and used for adjusting the temperature of the preparation area; the outside of furnace body still is provided with heating element and second temperature sensor in the position that corresponds with the dechlorination district, and heating element cooperates with second temperature sensor for adjust the temperature in dechlorination district.
3. The efficient and environment-friendly arsenic trichloride preparation device as claimed in claim 2, wherein: a discharging pipeline assembly is arranged at the bottom side of the collecting area and used for discharging liquid arsenic trichloride; a discharge control valve is arranged on a pipeline of the discharge pipeline assembly; the bottom of the collecting area is also provided with a deslagging pipeline assembly for deslagging, and a deslagging control valve is arranged on a pipeline of the deslagging pipeline assembly.
4. The efficient and environment-friendly arsenic trichloride production device according to claim 3, wherein: the upper part of the furnace body is also provided with a first gas pipeline component, and the gas inlet end of the first gas pipeline component is communicated with the furnace chamber of the furnace body; an exhaust valve is arranged on a pipeline of the first gas pipeline assembly; a safety valve is arranged between the furnace body and the exhaust valve on the pipeline of the first gas pipeline assembly; the first gas pipeline component is used for regulating the pressure of the furnace chamber and discharging tail gas; the upper position of the furnace body is also provided with a pressure sensor for monitoring the pressure of the furnace chamber.
5. The efficient and environment-friendly arsenic trichloride production apparatus according to claim 4, wherein: an arsenic feeding assembly is further arranged above the furnace body, and the discharge end of the arsenic feeding assembly is communicated with the furnace chamber; the arsenic charging assembly comprises an arsenic charging cavity, an arsenic discharging pipe is arranged at the bottom side of the arsenic charging cavity and used as a discharging end of the arsenic charging assembly, and an arsenic charging control valve is arranged between the arsenic discharging pipe and the furnace chamber; the top side of the arsenic charging cavity of the arsenic charging assembly is also provided with a charging cover plate for opening or closing a charging opening of the arsenic charging cavity; the charging cover plate is locked with the arsenic charging cavity through a quick connecting piece.
6. The efficient and environment-friendly arsenic trichloride production apparatus according to claim 5, wherein: the arsenic charging assembly is provided with a second gas pipeline assembly; an air inlet valve is arranged on a pipeline of the second gas pipeline assembly; the second gas pipeline component is used for introducing protective gas into the arsenic charging cavity and the furnace chamber.
7. The efficient and environment-friendly arsenic trichloride production apparatus according to claim 6, wherein: the chlorine gas supply assembly comprises a chlorine gas supply main pipe, a section of the chlorine gas supply main pipe, which is positioned outside the furnace body, is provided with a chlorine gas regulating valve and a chlorine gas flowmeter, and the tail end of the section of the chlorine gas supply main pipe, which is positioned in the furnace chamber, extends to the preparation area; the tail end of the chlorine gas supply main pipe is communicated with a plurality of chlorine gas supply branch pipes; the chlorine gas supply branch pipe is radially arranged by taking the tail end of the chlorine gas main pipe as the center; the chlorine gas supply branch pipes are uniformly distributed in a circle taking the tail end of the chlorine gas main pipe as the center; the chlorine gas supply branch pipe is positioned at a position close to the bottom side in the preparation area; one end of the chlorine gas supply branch pipe, which is far away from the tail end of the chlorine gas main pipe, is bent upwards towards the center to form an air outlet nozzle; the air outlet of the air outlet nozzle is not upward.
8. The efficient and environment-friendly arsenic trichloride production apparatus as claimed in claim 7, wherein: the arsenic trichloride preparation device further comprises a control module, and the control module is in communication connection with the air inlet valve, the air outlet valve, the pressure sensor, the arsenic feeding control valve, the chlorine regulating valve, the chlorine flowmeter, the cooling assembly, the first temperature sensor, the heating assembly and the second temperature sensor.
9. The efficient and environment-friendly arsenic trichloride production apparatus according to any one of claims 5 to 8, wherein: a furnace cover is arranged on the top side of the furnace body, and the furnace cover is fixed with the furnace body through a fastener; the arsenic charging assembly is arranged on the furnace cover.
10. The efficient and environment-friendly arsenic trichloride production apparatus according to any one of claims 1 to 8, wherein: the furnace body is also provided with an observation mirror at the position of the preparation area, and a cooling mechanism is arranged at the position of the observation mirror.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202222800616.XU CN219009925U (en) | 2022-10-24 | 2022-10-24 | High-efficient environment-friendly arsenic trichloride preparation facilities |
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