CN112176203A - Equipment and method for producing elemental arsenic by reducing white arsenic - Google Patents
Equipment and method for producing elemental arsenic by reducing white arsenic Download PDFInfo
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- CN112176203A CN112176203A CN202010813672.XA CN202010813672A CN112176203A CN 112176203 A CN112176203 A CN 112176203A CN 202010813672 A CN202010813672 A CN 202010813672A CN 112176203 A CN112176203 A CN 112176203A
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B30/00—Obtaining antimony, arsenic or bismuth
- C22B30/04—Obtaining arsenic
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
- C22B5/10—Dry methods smelting of sulfides or formation of mattes by solid carbonaceous reducing agents
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
- C22B5/12—Dry methods smelting of sulfides or formation of mattes by gases
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Abstract
An apparatus and a method for producing simple substance arsenic by reducing white arsenic, which comprises a spiral feeder, a sublimation furnace, a reduction furnace, a condenser, a first dust filter and a first vacuum pump which are sequentially communicated in a sealing way from left to right, the feed inlet of the screw feeder is connected with a bin, a first valve is arranged between the bin and the feed inlet of the screw feeder, the reduction furnace comprises a furnace body, the lower part of the furnace body is provided with an air inlet communicated with the sublimation furnace, the upper end of the furnace body is provided with an air charging hole and a feeding pipe, the feeding pipe is communicated with a charcoal bin, the charcoal bin is provided with an air exhaust hole, the feeding pipe is provided with a second valve, the condenser comprises a tank body, the tank body is provided with an electronic vibrator, the upper end detachably of the tank body is provided with a condensation pipe, and the condensation pipe is provided with a cooling water inlet and a cooling water outlet. The invention can improve the efficiency of sublimating the white arsenic into white arsenic steam and improve the efficiency of producing simple substance arsenic.
Description
Technical Field
The invention relates to the technical field of elemental arsenic production, in particular to equipment and a method for producing elemental arsenic by reducing white arsenic.
Background
Arsenic, which is a non-metallic element widely existing in nature, is a highly toxic substance but widely used in the industrial fields of alloy smelting, pesticides, medicines, pigments and the like, white arsenic is an oxide containing arsenic, has high toxicity, has a main component of arsenic trioxide, and is commonly used as a raw material for preparing simple substance arsenic in industrial production.
The method for preparing arsenic is mainly a hydrogen reduction method and a carbonizer method, and the preparation method comprises the steps of heating white arsenic in a sublimation furnace for sublimation, heating and reducing sublimed white arsenic steam in a reduction furnace to obtain arsenic steam, condensing the arsenic steam through a condenser to obtain simple substance arsenic.
Disclosure of Invention
The invention provides a device and a method for producing simple substance arsenic by reducing white arsenic, aiming at: the efficiency of white arsenic sublimation for white arsenic steam is improved, the efficiency of production simple substance arsenic is improved.
In order to achieve the purpose, the invention provides the following technical scheme:
an apparatus for producing elemental arsenic by reducing white arsenic, comprising a spiral feeder, a sublimation furnace, a reduction furnace, a condenser, a first dust filter and a first vacuum pump which are sequentially and hermetically communicated from left to right, wherein a feed inlet of the spiral feeder is connected with a bin, a first valve is arranged between the bin and the feed inlet of the spiral feeder, the reduction furnace comprises a furnace body, an air inlet communicated with the sublimation furnace is arranged at the lower part of the furnace body, an air charging hole and a feed pipe are arranged at the upper end of the furnace body, the feed pipe is communicated with a charcoal bin, an air exhaust hole is arranged on the charcoal bin, a second valve is arranged on the feed pipe, the condenser comprises a tank body, a material receiving hole is arranged at the lower end of the tank body, an electronic vibrator is arranged on the tank body, a condenser pipe is detachably arranged at the upper end of the tank body, and extends to the inside of the tank, and the condensation pipe is provided with a cooling water inlet and a cooling water outlet.
Furthermore, a partition board is horizontally arranged at the lower part of the furnace body, the partition board divides the interior of the furnace body into an upper cavity and a lower cavity, an air inlet at the lower part of the furnace body is positioned above the partition board, an ash cleaning port is arranged on the partition board and is communicated with the upper cavity and the lower cavity, a grid is arranged on the ash cleaning port, an ash discharging port is arranged at the bottom of the lower cavity, and the ash discharging port is connected with a third valve; the dust filter is characterized by further comprising a second vacuum pump and a second dust filter, wherein the inlet of the second dust filter is connected with the third valve through a pipeline, and the outlet of the second dust filter is connected with the second vacuum pump.
Furthermore, the middle part of the partition board is arranged in a concave mode, and the ash removal opening is formed in the middle of the partition board.
Furthermore, an upper cover is detachably arranged at the upper end of the furnace body, a sealing strip is arranged at the joint of the furnace body and the upper cover, the feeding pipe is arranged on the upper cover, and a first cooling jacket is arranged on the upper cover.
Further, the junction of top cap with the jar body is provided with the sealing strip, be provided with the second cooling jacket on the top cap.
A method of producing elemental arsenic using the apparatus for producing elemental arsenic by reduction of white arsenic described above, comprising:
(1) conveying the white arsenic to a bin of a screw feeder for standby;
(2) opening cooling water inlet and outlet valves on a condensation pipe of a condenser, and adding 50-100 kg of charcoal into a reduction furnace;
(3) pumping vacuum of the sublimation furnace, the reduction furnace and the condenser through a vacuum pump to enable the vacuum degree to reach 10-100 Pa;
(4) after the vacuum degree of the whole system is pumped to 10-100 Pa, the vacuum pump is closed, and protective gas is filled into the system to enable the whole pressure of the system to be below 0.05 MPa;
(5) starting a heating program of the sublimation furnace and the reduction furnace, and stably heating at a speed of 10-20 ℃/min to ensure that the overall pressure of the system is lower than 0.1 MPa;
(6) starting a spiral feeder after the temperature of the sublimation furnace rises to 300-600 ℃ and the temperature of the reduction furnace reaches 500-800 ℃, adjusting a frequency modulator to be 20-30 Hz, feeding the sublimation furnace at a rate of 1.5-2.5 kg/min, and keeping the vacuum degree of the system at 10-100 Pa;
(7) keeping the temperature of a sublimation furnace at 300-600 ℃, keeping the temperature of a reduction furnace at 500-800 ℃, keeping the temperature of a condenser at 50-250 ℃, and continuously sublimating, reducing and condensing the materials;
(8) after 300kg of material is fed, vacuumizing a charcoal bin of a reduction furnace, starting a charcoal bin valve when the pressure reaches 10-100 Pa, supplementing charcoal into the reduction furnace, and supplementing 50-100 kg of charcoal once;
(9) after feeding 400-500 kg, starting an electronic vibrator, and intermittently knocking the wall of the condenser to enable the condensed elemental arsenic to fall to the bottom of the condenser;
(10) after feeding 800-1000 kg, stopping feeding, keeping the system at a vacuum degree of 10-100 Pa, continuously keeping the sublimation furnace and the reduction furnace at a temperature of 500-800 ℃ for 2h, continuously carrying out reduction and condensation, and stopping heating the sublimation furnace and the reduction furnace when the pressure of the vacuum pump system is closed and is not obviously increased;
(11) after the condenser temperature drops to below 50 ℃, begin the ejection of compact, during the ejection of compact, open the top cap of condenser earlier, then hang out the top cap of condenser with the driving, collect the back packing with the simple substance arsenic on the top cap condenser pipe and put in storage, the sample is sent the laboratory analysis, will drop condenser bottom simple substance arsenic through the discharge gate of condenser lower extreme simultaneously and take out, the sample is sent the laboratory analysis.
Further, in the step (11), top covers of a plurality of condensers are prepared, when discharging is carried out, another top cover is immediately covered after the top cover of the condenser is lifted out by a travelling crane, and the steps (1) to (10) are repeated.
Further, in the step (11), the top cover of the condenser is lifted by a crane during discharging, and then the lower part of the condenser is maintained in a negative pressure state.
A method of producing elemental arsenic using the apparatus for producing elemental arsenic by reduction of white arsenic described above, comprising:
(1) conveying the white arsenic to a bin of a screw feeder for standby;
(2) opening cooling water inlet and outlet valves on a condensation pipe of the condenser;
(3) pumping vacuum of the sublimation furnace, the reduction furnace and the condenser through a vacuum pump to enable the vacuum degree to reach 10-100 Pa;
(4) after the vacuum degree of the whole system is pumped to 10-100 Pa, the vacuum pump is closed, and reducing gas is filled into the system to enable the whole pressure of the system to be below 0.05 MPa;
(5) starting a heating program of the sublimation furnace and the reduction furnace, stably heating at a speed of 10-20 ℃/min, and stopping filling reducing gas when the pressure is higher than 0.1 MPa;
(6) starting a spiral feeder after the temperature of the sublimation furnace rises to 300-600 ℃ and the temperature of the reduction furnace reaches 500-800 ℃, adjusting a frequency modulator to be 20-30 Hz, feeding the sublimation furnace at a rate of 1.5-2.5 kg/min, and keeping the vacuum degree of the system at 10-100 Pa;
(7) keeping the temperature of a sublimation furnace at 300-600 ℃, keeping the temperature of a reduction furnace at 500-800 ℃, keeping the temperature of a condenser at 50-250 ℃, and continuously sublimating, reducing and condensing the materials;
(8) after 300kg of feeding, replenishing reducing gas into the reducing furnace, and ensuring that the pressure in the furnace is not higher than 0.1MPa during replenishing;
(9) after feeding 400-500 kg, starting an electronic vibrator, and intermittently knocking the wall of the condenser to enable the condensed elemental arsenic to fall to the bottom of the condenser;
(10) after feeding 800-1000 kg, stopping feeding, keeping the system at a vacuum degree of 10-100 Pa, continuously keeping the sublimation furnace and the reduction furnace at a temperature of 500-800 ℃ for 2h, continuously carrying out reduction and condensation, and stopping heating the sublimation furnace and the reduction furnace when the pressure of the vacuum pump system is closed and is not obviously increased;
(11) after the condenser temperature drops to below 50 ℃, begin the ejection of compact, during the ejection of compact, open the top cap of condenser earlier, then hang out the top cap of condenser with the driving, collect the back packing with the simple substance arsenic on the top cap condenser pipe and put in storage, the sample is sent the laboratory analysis, will drop condenser bottom simple substance arsenic through the discharge gate of condenser lower extreme simultaneously and take out, the sample is sent the laboratory analysis.
Further, in the step (11), top covers of a plurality of condensers are prepared, when discharging is carried out, another top cover is immediately covered after the top cover of the condenser is lifted out by a travelling crane, and the steps (1) to (10) are repeated.
Compared with the prior art, the invention has the beneficial effects that:
1. the whole device is subjected to vacuum pumping operation during white arsenic reduction, the internal pressure is low, the sublimation point of the white arsenic in a sublimation furnace is reduced, the sublimation efficiency of the white arsenic is improved, the efficiency of producing elemental arsenic is further improved, the first dust filter can filter condensed arsenic vapor, and the arsenic vapor is prevented from entering the first vacuum pump, damaging equipment and polluting the environment;
2. because the whole device is hermetically connected, continuous feeding and continuous production can be realized, a large amount of materials can be reduced at one time, and the production efficiency is improved;
3. the whole device can be reduced by carbon, and can also be reduced by reducing gas, such as hydrogen or carbon monoxide, so that the universality of the equipment is improved;
4. when charcoal powder in the reducing furnace needs to be cleaned, charcoal ash on the partition plate can be pumped into the second dust filter through the ash cleaning port and the grating by the second vacuum pump, the method is simple and convenient, and the ash cleaning efficiency is high.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are only embodiments of the present application, and it is obvious for those skilled in the art to obtain other drawings based on the provided drawings without creative efforts.
FIG. 1 is a schematic structural diagram of one embodiment of the present invention;
FIG. 2 is a schematic view of the reduction furnace of FIG. 1;
FIG. 3 is a cross-sectional view taken along A-A of FIG. 2;
FIG. 4 is a schematic view of the condenser of FIG. 1;
fig. 5 is a top view of fig. 4.
In the figure: 10. the device comprises a screw feeder, 1001, a storage bin, 1002, a first valve, 20, a sublimation furnace, 2001, a first cooling pipe, 30, a reduction furnace, 3001, a furnace body, 3002, an upper cover, 30021, a gas filling hole, 3003, a cooling jacket, 3004, a feeding pipe, 3005, a second valve, 3006, a charcoal bin, 30061, a gas extraction opening, 3007, a partition plate, 30071, a dust removal opening, 3008, a lower cavity, 3009, a third valve, 3010, a grid, 40, a condenser, 4001, a tank body, 4002, a top cover, 4003, a second cooling jacket, 4004, a condensation pipe, 50, a first dust filter, 60, a first vacuum pump, 70, a second vacuum pump, 80 and a second dust filter.
Detailed Description
In order to make those skilled in the art better understand the technical solution of the present invention, the technical solution in the embodiment of the present invention will be clearly and completely described below with reference to the drawings in the embodiment of the present invention.
Example 1:
as shown in fig. 1, the present invention provides an apparatus for producing elemental arsenic by reducing white arsenic, comprising a screw feeder 10, a sublimation furnace 20, a reduction furnace 30, a condenser 40, a first dust filter 50 and a first vacuum pump 60, which are hermetically connected from left to right, wherein a feed port of the screw feeder 10 is connected to a storage bin 1001, a first valve 1002 is disposed between the storage bin 1001 and the feed port of the screw feeder 10 to open and close the storage bin 1001 and the feed port of the screw feeder 10, the reduction furnace 30 comprises a furnace body 3001, an air inlet communicated with the sublimation furnace 20 is disposed at a lower portion of the furnace body 3001, an air inlet 30021 and a feed pipe 3004 are disposed at an upper end of the furnace body 3001, the feed pipe 3004 is communicated to a charcoal bin 3006, an air outlet 30061 is disposed on the charcoal bin 3006 to evacuate the charcoal bin 3006 through the air outlet 30061, a second valve 3005 is disposed on the feed pipe 3004 to open and close the charcoal bin 3006 and, condenser 40 is provided with the material receiving port including jar body 4001, jar body 4001's lower extreme, is provided with the electronic shaker on jar body 4001, and jar body 4001's upper end detachably is provided with condenser pipe 4004, and condenser pipe 4004 extends to jar body 4001's inside, is provided with cooling water inlet and cooling water export on the condenser pipe 4004, cools off condenser pipe 4004 through cooling water inlet and cooling water export and stretches into jar body 4001 inside pipe wall, is used for with arsenic steam condensation crystallization.
As shown in fig. 2 and 3, in this embodiment, a partition 3007 is horizontally disposed at the lower part of the furnace body 3001, the partition 3007 divides the interior of the furnace body 3001 into an upper cavity and a lower cavity 3008, an air inlet at the lower part of the furnace body 3001 is located above the partition 3007, an ash removal port 30071 is disposed on the partition 3007, the ash removal port 30071 communicates the upper cavity with the lower cavity 3008, a grid 3001 is disposed on the ash removal port 30071, an ash discharge port is disposed at the bottom of the lower cavity 3008, and the ash discharge port is connected to a third valve 3009; the reduction furnace further comprises a second vacuum pump 70 and a second dust filter 80, an inlet of the second dust filter 80 is connected with a third valve 3009 through a pipeline, an outlet of the second dust filter 80 is connected with the second vacuum pump 70, and when charcoal powder in the reduction furnace body 3001 needs to be cleaned, charcoal ash on the partition 3007 can be pumped into the second dust filter 80 through the ash cleaning port 30071 and the grating 3001 through the second vacuum pump 70. .
In this embodiment, the middle of the partition 3007 is recessed, and the ash removal opening 30071 is formed in the middle of the partition 3007, so that charcoal ash can flow to the middle of the partition 3007 and fall through the ash removal opening 30071 during use, and the partition 3007 is more convenient to clean.
As shown in fig. 4, in this embodiment, the upper end of the furnace body 3001 is detachably provided with the upper cover 3002, which facilitates opening the upper cover 3002 to clean and maintain the inside of the furnace body 3001, the joint between the furnace body 3001 and the upper cover 3002 is provided with a sealing strip, the feeding pipe is arranged on the upper cover 3002, the upper cover 3002 is provided with the first cooling jacket 3003, and the first cooling jacket 3003 cools the sealing strip at the joint between the furnace body 3001 and the upper cover 3002 to prevent deformation and influence the sealing performance of the whole device.
In this embodiment, the joint of top cover 4002 and jar body 4001 is provided with the sealing strip, is provided with second cooling jacket 4003 on top cover 4002, and second cooling jacket 4003 cools down the sealing strip of the joint of top cover 4002 and jar body 4001, prevents that it from taking place to warp and influencing the leakproofness of whole device.
As shown in fig. 4 and 5. In this embodiment, condenser pipe 4004 sets up a plurality ofly according to circular even interval distribution, can improve the area of contact of condenser pipe 4004 and arsenic steam, and single condenser pipe 4004 heat exchange efficiency is higher, has improved the condensation efficiency of arsenic steam, and then has improved production efficiency.
The invention can use carbon to reduce white arsenic, and adopts the following method:
a method of producing elemental arsenic using the apparatus for producing elemental arsenic by reduction of white arsenic described above, comprising:
(1) conveying the white arsenic to a bin of a screw feeder for standby;
(2) opening cooling water inlet and outlet valves on a condensation pipe of the condenser, and adding 50kg of charcoal into the reduction furnace;
(3) pumping the vacuum of the sublimation furnace, the reduction furnace and the condenser by using a vacuum pump to ensure that the vacuum degree reaches 10 Pa;
(4) after the vacuum degree of the whole system is pumped to 10Pa, the vacuum pump is closed, and protective gas is filled into the system to ensure that the whole pressure of the system is below 0.05 MPa;
(5) starting a heating program of the sublimation furnace and the reduction furnace, and stably heating at a speed of 10 ℃/min to ensure that the overall pressure of the system is lower than 0.1 MPa;
(6) starting a spiral feeder after the temperature of the sublimation furnace rises to 300 ℃ and the temperature of the reduction furnace reaches 500 ℃, adjusting a frequency modulator to be 20Hz, and feeding the sublimation furnace at a speed of 1.5/min to keep the vacuum degree of the system at 10 Pa;
(7) keeping the temperature of the sublimation furnace at 300 ℃, the temperature of the reduction furnace at 500 ℃, and the temperature of the condenser at 50 ℃ so as to continuously sublimate, reduce and condense the materials;
(8) after 300kg of material is fed, vacuumizing a charcoal bin of a reduction furnace until the pressure reaches 10Pa, opening a charcoal bin valve, supplementing charcoal into the reduction furnace, and supplementing 50kg of charcoal once;
(9) after 400kg of material is fed, starting an electronic vibrator, and intermittently knocking the wall of the condenser to enable condensed elemental arsenic to fall to the bottom of the condenser, so that the elemental arsenic on the wall of the condenser is prevented from being accumulated too much and too thick and cannot fall off in the later period;
(10) after feeding 800kg, stopping feeding, keeping the system at a vacuum degree of 10Pa, continuously keeping the sublimation furnace and the reduction furnace at a temperature of 500 ℃ for 2h, continuously carrying out reduction and condensation, and stopping heating the sublimation furnace and the reduction furnace when the pressure of the vacuum pump system is closed and is not obviously increased;
(11) after the condenser temperature drops to below 50 ℃, begin the ejection of compact, during the ejection of compact, open the top cap of condenser earlier, then hang out the top cap of condenser with the driving, collect the back packing with the simple substance arsenic on the top cap condenser pipe and put in storage, the sample is sent the laboratory analysis, will drop condenser bottom simple substance arsenic through the discharge gate of condenser lower extreme simultaneously and take out, the sample is sent the laboratory analysis.
In order to reduce the discharging time, in the step (11), top covers of a plurality of condensers are prepared, during discharging, after the top covers of the condensers are lifted out by a travelling crane, another top cover is immediately covered, and the steps (1) to (10) are repeated, so that when the elemental arsenic on the top cover condenser pipe is collected, the other white arsenic can be continuously reduced, the waiting time is shortened, and the production efficiency is improved.
In this embodiment, in the step (11), the top cover of the condenser is lifted by the traveling crane during discharging, and then the lower part of the condenser is maintained in a negative pressure state, so that the gas in the incomplete reduction apparatus is prevented from leaking through the upper end opening of the condenser after the top cover of the condenser is lifted by the traveling crane.
The invention can also use reducing gas to reduce white arsenic, and adopts the following method:
a method of producing elemental arsenic using the apparatus for producing elemental arsenic by reduction of white arsenic described above, comprising:
(1) conveying the white arsenic to a bin of a screw feeder for standby;
(2) opening cooling water inlet and outlet valves on a condensation pipe of the condenser;
(3) pumping the vacuum of the sublimation furnace, the reduction furnace and the condenser by using a vacuum pump to ensure that the vacuum degree reaches 10 Pa;
(4) after the vacuum degree of the whole system is pumped to 10Pa, the vacuum pump is closed, reducing gas, such as hydrogen gas or carbon monoxide gas and the like, is filled into the system, and the whole pressure of the system is below 0.05 MPa;
(5) starting a heating program of the sublimation furnace and the reduction furnace, stably heating at the speed of 10 ℃/min, and stopping filling the reduction gas when the pressure is higher than 0.1 MPa;
(6) after the temperature of the sublimation furnace rises to 300 ℃ and the temperature of the reduction furnace reaches 500 ℃, starting a spiral feeder, adjusting a frequency converter to be 20Hz, feeding the sublimation furnace at a rate of 1.5 kg/min, and keeping the vacuum degree of the system at 10 Pa;
(7) keeping the temperature of the sublimation furnace at 300 ℃, the temperature of the reduction furnace at 500 ℃, and the temperature of the condenser at 50 ℃ so as to continuously sublimate, reduce and condense the materials;
(8) after 300kg of feeding, replenishing reducing gas into the reducing furnace, and ensuring that the pressure in the furnace is not higher than 0.1MPa during replenishing;
(9) after 400kg of material is fed, starting an electronic vibrator, and intermittently knocking the wall of the condenser to enable the condensed elemental arsenic to fall to the bottom of the condenser;
(10) after feeding 800kg, stopping feeding, keeping the system at a vacuum degree of 10Pa, continuously keeping the sublimation furnace and the reduction furnace at a temperature of 500 ℃ for 2h, continuously carrying out reduction and condensation, and stopping heating the sublimation furnace and the reduction furnace when the pressure of the vacuum pump system is closed and is not obviously increased;
(11) after the condenser temperature drops to below 50 ℃, begin the ejection of compact, during the ejection of compact, open the top cap of condenser earlier, then hang out the top cap of condenser with the driving, collect the back packing with the simple substance arsenic on the top cap condenser pipe and put in storage, the sample is sent the laboratory analysis, will drop condenser bottom simple substance arsenic through the discharge gate of condenser lower extreme simultaneously and take out, the sample is sent the laboratory analysis.
Further, in the step (11), top covers of a plurality of condensers are prepared, when discharging is carried out, another top cover is immediately covered after the top cover of the condenser is lifted out by a travelling crane, and the steps (1) to (10) are repeated.
In the actual use process, the whole device carries out vacuumizing operation during white arsenic reduction, so that the sublimation point of the white arsenic in a sublimation furnace is reduced, the sublimation efficiency of the white arsenic is improved, and the efficiency of producing simple substance arsenic is further improved; the whole device is hermetically connected, so that continuous feeding and continuous production can be realized, a large amount of materials can be reduced at one time, and the production efficiency is improved; the whole device can be reduced by carbon, and can also be reduced by reducing gas, such as hydrogen or carbon monoxide, so that the universality of the equipment is improved; when charcoal powder in the reducing furnace needs to be cleaned, charcoal ash on the partition plate can be pumped into the second dust filter through the ash cleaning port and the grating by the second vacuum pump, the method is simple and convenient, and the ash cleaning efficiency is high.
Example 2:
this example used the same apparatus for producing elemental arsenic by reduction of white arsenic as in example 1 and used the following method for reducing white arsenic:
white arsenic is reduced by using carbon, and the following method is adopted:
a method of producing elemental arsenic using the apparatus for producing elemental arsenic by reduction of white arsenic described above, comprising:
(1) conveying the white arsenic to a bin of a screw feeder for standby;
(2) opening cooling water inlet and outlet valves on a condensing pipe of a condenser, and adding 100kg of charcoal into a reducing furnace;
(3) pumping the vacuum of the sublimation furnace, the reduction furnace and the condenser by using a vacuum pump to ensure that the vacuum degree reaches 100 Pa;
(4) after the vacuum degree of the whole system is pumped to 100Pa, the vacuum pump is closed, and protective gas is filled into the system to ensure that the whole pressure of the system is below 0.05 MPa;
(5) starting a heating program of the sublimation furnace and the reduction furnace, and stably heating at the speed of 20 ℃/min to ensure that the overall pressure of the system is lower than 0.1 MPa;
(6) starting a spiral feeder after the temperature of the sublimation furnace rises to 600 ℃ and the temperature of the reduction furnace reaches 800 ℃, adjusting a frequency converter to be 30Hz, feeding the sublimation furnace at the speed of 2.5 kg/min, and keeping the vacuum degree of the system at 100 Pa;
(7) keeping the temperature of the sublimation furnace at 600 ℃, the temperature of the reduction furnace at 800 ℃, and the temperature of the condenser at 250 ℃ so that the materials are continuously sublimated, reduced and condensed;
(8) after 300kg of material is fed, vacuumizing a charcoal bin of a reduction furnace until the pressure reaches 100Pa, opening a charcoal bin valve, supplementing charcoal into the reduction furnace, and supplementing 100kg of charcoal once;
(9) after 500kg of feed is fed, starting an electronic vibrator, and intermittently knocking the wall of the condenser to enable condensed elemental arsenic to fall to the bottom of the condenser;
(10) after 1000kg of material is fed, stopping feeding, keeping the system at a vacuum degree of 100Pa, continuously keeping the sublimation furnace and the reduction furnace at a temperature of 800 ℃ for 2h, continuously carrying out reduction and condensation, and stopping heating the sublimation furnace and the reduction furnace when the pressure of the vacuum pump system is closed and is not obviously increased;
(11) after the condenser temperature drops to below 50 ℃, begin the ejection of compact, during the ejection of compact, open the top cap of condenser earlier, then hang out the top cap of condenser with the driving, collect the back packing with the simple substance arsenic on the top cap condenser pipe and put in storage, the sample is sent the laboratory analysis, will drop condenser bottom simple substance arsenic through the discharge gate of condenser lower extreme simultaneously and take out, the sample is sent the laboratory analysis.
In this embodiment, in the step (11), the top cover of the condenser is lifted by the traveling crane during discharging, and then the lower part of the condenser is maintained in a negative pressure state, so that the gas in the incomplete reduction apparatus is prevented from leaking through the upper end opening of the condenser after the top cover of the condenser is lifted by the traveling crane.
When reducing white arsenic by using reducing gas, the following method is adopted:
a method of producing elemental arsenic using the apparatus for producing elemental arsenic by reduction of white arsenic described above, comprising:
(1) conveying the white arsenic to a bin of a screw feeder for standby;
(2) opening cooling water inlet and outlet valves on a condensation pipe of the condenser;
(3) pumping the vacuum of the sublimation furnace, the reduction furnace and the condenser by using a vacuum pump to ensure that the vacuum degree reaches 100 Pa;
(4) after the vacuum degree of the whole system is pumped to 100Pa, the vacuum pump is closed, reducing gas, such as hydrogen gas or carbon monoxide gas and the like, is filled into the system, and the whole pressure of the system is below 0.05 MPa;
(5) starting a heating program of the sublimation furnace and the reduction furnace, stably heating at the speed of 20 ℃/min, and stopping filling the reduction gas when the pressure is higher than 0.1 MPa;
(6) starting a spiral feeder after the temperature of the sublimation furnace rises to 600 ℃ and the temperature of the reduction furnace reaches 800 ℃, adjusting a frequency converter to be 30Hz, feeding the sublimation furnace at the speed of 2.5 kg/min, and keeping the vacuum degree of the system at 100 Pa;
(7) keeping the temperature of the sublimation furnace at 600 ℃, the temperature of the reduction furnace at 800 ℃, and the temperature of the condenser at 250 ℃ so that the materials are continuously sublimated, reduced and condensed;
(8) after 300kg of feeding, replenishing reducing gas into the reducing furnace, and ensuring that the pressure in the furnace is not higher than 0.1MPa during replenishing;
(9) after 500kg of feed is fed, starting an electronic vibrator, and intermittently knocking the wall of the condenser to enable condensed elemental arsenic to fall to the bottom of the condenser;
(10) after 1000kg of material is fed, stopping feeding, keeping the system at a vacuum degree of 100Pa, continuously keeping the sublimation furnace and the reduction furnace at a temperature of 800 ℃ for 2h, continuously carrying out reduction and condensation, and stopping heating the sublimation furnace and the reduction furnace when the pressure of the vacuum pump system is closed and is not obviously increased;
(11) after the condenser temperature drops to below 50 ℃, begin the ejection of compact, during the ejection of compact, open the top cap of condenser earlier, then hang out the top cap of condenser with the driving, collect the back packing with the simple substance arsenic on the top cap condenser pipe and put in storage, the sample is sent the laboratory analysis, will drop condenser bottom simple substance arsenic through the discharge gate of condenser lower extreme simultaneously and take out, the sample is sent the laboratory analysis.
Example 3:
this example used the same apparatus for producing elemental arsenic by reduction of white arsenic as in example 1 and used the following method for reducing white arsenic:
white arsenic is reduced by using carbon, and the following method is adopted:
a method of producing elemental arsenic using the apparatus for producing elemental arsenic by reduction of white arsenic described above, comprising:
(1) conveying the white arsenic to a bin of a screw feeder for standby;
(2) opening cooling water inlet and outlet valves on a condensation pipe of the condenser, and adding 70kg of charcoal into the reduction furnace;
(3) pumping the vacuum of the sublimation furnace, the reduction furnace and the condenser by using a vacuum pump to ensure that the vacuum degree reaches 50 Pa;
(4) after the vacuum degree of the whole system is pumped to 50Pa, the vacuum pump is closed, and protective gas is filled into the system to ensure that the whole pressure of the system is below 0.05 MPa;
(5) starting a heating program of the sublimation furnace and the reduction furnace, and stably heating at a speed of 15 ℃/min to ensure that the overall pressure of the system is lower than 0.1 MPa;
(6) starting a spiral feeder after the temperature of the sublimation furnace rises to 450 ℃ and the temperature of the reduction furnace reaches 600 ℃, adjusting a frequency modulator to be 25Hz, and feeding the material to the sublimation furnace at the speed of 2 kg/min to keep the vacuum degree of the system at 50 Pa;
(7) keeping the temperature of the sublimation furnace at 450 ℃, the temperature of the reduction furnace at 600 ℃, and the temperature of the condenser at 150 ℃ so as to continuously sublimate, reduce and condense the materials;
(8) after 300kg of material is fed, vacuumizing a charcoal bin of a reduction furnace until the pressure reaches 50Pa, opening a charcoal bin valve, supplementing charcoal into the reduction furnace, and supplementing 70kg of charcoal once;
(9) after 450kg of feed is fed, starting an electronic vibrator, and intermittently knocking the wall of the condenser to enable the condensed elemental arsenic to fall to the bottom of the condenser;
(10) after feeding 900kg, stopping feeding, keeping the system at a vacuum degree of 50Pa, continuously keeping the sublimation furnace and the reduction furnace at a temperature of 600 ℃ for 2h, continuously carrying out reduction and condensation, and stopping heating the sublimation furnace and the reduction furnace when the pressure of the vacuum pump system is closed and is not obviously increased;
(11) after the condenser temperature drops to below 50 ℃, begin the ejection of compact, during the ejection of compact, open the top cap of condenser earlier, then hang out the top cap of condenser with the driving, collect the back packing with the simple substance arsenic on the top cap condenser pipe and put in storage, the sample is sent the laboratory analysis, will drop condenser bottom simple substance arsenic through the discharge gate of condenser lower extreme simultaneously and take out, the sample is sent the laboratory analysis.
In this embodiment, in the step (11), the top cover of the condenser is lifted by the traveling crane during discharging, and then the lower part of the condenser is maintained in a negative pressure state, so that the gas in the incomplete reduction apparatus is prevented from leaking through the upper end opening of the condenser after the top cover of the condenser is lifted by the traveling crane.
When reducing white arsenic by using reducing gas, the following method is adopted:
a method of producing elemental arsenic using the apparatus for producing elemental arsenic by reduction of white arsenic described above, comprising:
(1) conveying the white arsenic to a bin of a screw feeder for standby;
(2) opening cooling water inlet and outlet valves on a condensation pipe of the condenser;
(3) pumping the vacuum of the sublimation furnace, the reduction furnace and the condenser by using a vacuum pump to ensure that the vacuum degree reaches 50 Pa;
(4) after the vacuum degree of the whole system is pumped to 50Pa, the vacuum pump is closed, reducing gas, such as hydrogen gas or carbon monoxide gas and the like, is filled into the system, and the whole pressure of the system is below 0.05 MPa;
(5) starting a heating program of the sublimation furnace and the reduction furnace, stably heating at a speed of 15 ℃/min, and stopping filling the reduction gas when the pressure is higher than 0.1 MPa;
(6) starting a spiral feeder after the temperature of the sublimation furnace rises to 450 ℃ and the temperature of the reduction furnace reaches 600 ℃, adjusting a frequency modulator to be 25Hz, and feeding the material to the sublimation furnace at the speed of 2 kg/min to keep the vacuum degree of the system at 50 Pa;
(7) keeping the temperature of the sublimation furnace at 450 ℃, the temperature of the reduction furnace at 600 ℃, and the temperature of the condenser at 150 ℃ so as to continuously sublimate, reduce and condense the materials;
(8) after 300kg of feeding, replenishing reducing gas into the reducing furnace, and ensuring that the pressure in the furnace is not higher than 0.1MPa during replenishing;
(9) after 450kg of feed is fed, starting an electronic vibrator, and intermittently knocking the wall of the condenser to enable the condensed elemental arsenic to fall to the bottom of the condenser;
(10) after feeding 900kg, stopping feeding, keeping the system at a vacuum degree of 50Pa, continuously keeping the sublimation furnace and the reduction furnace at a temperature of 600 ℃ for 2h, continuously carrying out reduction and condensation, and stopping heating the sublimation furnace and the reduction furnace when the pressure of the vacuum pump system is closed and is not obviously increased;
(11) after the condenser temperature drops to below 50 ℃, begin the ejection of compact, during the ejection of compact, open the top cap of condenser earlier, then hang out the top cap of condenser with the driving, collect the back packing with the simple substance arsenic on the top cap condenser pipe and put in storage, the sample is sent the laboratory analysis, will drop condenser bottom simple substance arsenic through the discharge gate of condenser lower extreme simultaneously and take out, the sample is sent the laboratory analysis.
Example 4:
this example used the same apparatus for producing elemental arsenic by reduction of white arsenic as in example 1 and used the following method for reducing white arsenic:
white arsenic is reduced by using carbon, and the following method is adopted:
a method of producing elemental arsenic using the apparatus for producing elemental arsenic by reduction of white arsenic described above, comprising:
(1) conveying the white arsenic to a bin of a screw feeder for standby;
(2) opening cooling water inlet and outlet valves on a condensation pipe of the condenser, and adding 50kg of charcoal into the reduction furnace;
(3) pumping the vacuum of the sublimation furnace, the reduction furnace and the condenser by using a vacuum pump to ensure that the vacuum degree reaches 30 Pa;
(4) after the vacuum degree of the whole system is pumped to 30Pa, the vacuum pump is closed, and protective gas is filled into the system to ensure that the whole pressure of the system is below 0.05 MPa;
(5) starting a heating program of the sublimation furnace and the reduction furnace, and stably heating at a speed of 10 ℃/min to ensure that the overall pressure of the system is lower than 0.1 MPa;
(6) starting a spiral feeder after the temperature of the sublimation furnace rises to 300 ℃ and the temperature of the reduction furnace reaches 500 ℃, adjusting a frequency modulator to be 20Hz, and feeding the sublimation furnace at a speed of 1.5/min to keep the vacuum degree of the system at 30 Pa;
(7) keeping the temperature of the sublimation furnace at 300 ℃, the temperature of the reduction furnace at 500 ℃, and the temperature of the condenser at 50 ℃ so as to continuously sublimate, reduce and condense the materials;
(8) after 300kg of material is fed, vacuumizing a charcoal bin of a reduction furnace until the pressure reaches 30Pa, opening a charcoal bin valve, supplementing charcoal into the reduction furnace, and supplementing 50kg of charcoal once;
(9) after 400kg of material is fed, starting an electronic vibrator, and intermittently knocking the wall of the condenser to enable the condensed elemental arsenic to fall to the bottom of the condenser;
(10) after feeding 800kg, stopping feeding, keeping the system at a vacuum degree of 30Pa, continuously keeping the sublimation furnace and the reduction furnace at a temperature of 500 ℃ for 2h, continuously carrying out reduction and condensation, and stopping heating the sublimation furnace and the reduction furnace when the pressure of the vacuum pump system is closed and is not obviously increased;
(11) after the condenser temperature drops to below 50 ℃, begin the ejection of compact, during the ejection of compact, open the top cap of condenser earlier, then hang out the top cap of condenser with the driving, collect the back packing with the simple substance arsenic on the top cap condenser pipe and put in storage, the sample is sent the laboratory analysis, will drop condenser bottom simple substance arsenic through the discharge gate of condenser lower extreme simultaneously and take out, the sample is sent the laboratory analysis.
Reducing white arsenic by using a reducing gas, and adopting the following method:
a method of producing elemental arsenic using the apparatus for producing elemental arsenic by reduction of white arsenic described above, comprising:
(1) conveying the white arsenic to a bin of a screw feeder for standby;
(2) opening cooling water inlet and outlet valves on a condensation pipe of the condenser;
(3) pumping the vacuum of the sublimation furnace, the reduction furnace and the condenser by using a vacuum pump to ensure that the vacuum degree reaches 30 Pa;
(4) after the vacuum degree of the whole system is pumped to 30Pa, the vacuum pump is closed, reducing gas, such as hydrogen gas or carbon monoxide gas and the like, is filled into the system, and the whole pressure of the system is below 0.05 MPa;
(5) starting a heating program of the sublimation furnace and the reduction furnace, stably heating at the speed of 10 ℃/min, and stopping filling the reduction gas when the pressure is higher than 0.1 MPa;
(6) after the temperature of the sublimation furnace rises to 300 ℃ and the temperature of the reduction furnace reaches 500 ℃, starting a spiral feeder, adjusting a frequency converter to be 20Hz, feeding the sublimation furnace at a rate of 1.5 kg/min, and keeping the vacuum degree of the system at 30 Pa;
(7) keeping the temperature of the sublimation furnace at 300 ℃, the temperature of the reduction furnace at 500 ℃, and the temperature of the condenser at 50 ℃ so as to continuously sublimate, reduce and condense the materials;
(8) after 300kg of feeding, replenishing reducing gas into the reducing furnace, and ensuring that the pressure in the furnace is not higher than 0.1MPa during replenishing;
(9) after 400kg of material is fed, starting an electronic vibrator, and intermittently knocking the wall of the condenser to enable the condensed elemental arsenic to fall to the bottom of the condenser;
(10) after feeding 800kg, stopping feeding, keeping the system at a vacuum degree of 30Pa, continuously keeping the sublimation furnace and the reduction furnace at a temperature of 500 ℃ for 2h, continuously carrying out reduction and condensation, and stopping heating the sublimation furnace and the reduction furnace when the pressure of the vacuum pump system is closed and is not obviously increased;
(11) after the condenser temperature drops to below 50 ℃, begin the ejection of compact, during the ejection of compact, open the top cap of condenser earlier, then hang out the top cap of condenser with the driving, collect the back packing with the simple substance arsenic on the top cap condenser pipe and put in storage, the sample is sent the laboratory analysis, will drop condenser bottom simple substance arsenic through the discharge gate of condenser lower extreme simultaneously and take out, the sample is sent the laboratory analysis.
Example 5:
this example used the same apparatus for producing elemental arsenic by reduction of white arsenic as in example 1 and used the following method for reducing white arsenic:
white arsenic is reduced by using carbon, and the following method is adopted:
a method of producing elemental arsenic using the apparatus for producing elemental arsenic by reduction of white arsenic described above, comprising:
(1) conveying the white arsenic to a bin of a screw feeder for standby;
(2) opening cooling water inlet and outlet valves on a condensation pipe of the condenser, and adding 50kg of charcoal into the reduction furnace;
(3) pumping the vacuum of the sublimation furnace, the reduction furnace and the condenser by using a vacuum pump to ensure that the vacuum degree reaches 50 Pa;
(4) after the vacuum degree of the whole system is pumped to 50Pa, the vacuum pump is closed, and protective gas is filled into the system to ensure that the whole pressure of the system is below 0.05 MPa;
(5) starting a heating program of the sublimation furnace and the reduction furnace, and stably heating at a speed of 10 ℃/min to ensure that the overall pressure of the system is lower than 0.1 MPa;
(6) starting a spiral feeder after the temperature of the sublimation furnace rises to 300 ℃ and the temperature of the reduction furnace reaches 500 ℃, adjusting a frequency modulator to be 20Hz, and feeding the sublimation furnace at a speed of 1.5/min to keep the vacuum degree of the system at 50 Pa;
(7) keeping the temperature of the sublimation furnace at 300 ℃, the temperature of the reduction furnace at 500 ℃, and the temperature of the condenser at 50 ℃ so as to continuously sublimate, reduce and condense the materials;
(8) after 300kg of material is fed, vacuumizing a charcoal bin of a reduction furnace until the pressure reaches 50Pa, opening a charcoal bin valve, supplementing charcoal into the reduction furnace, and supplementing 50kg of charcoal once;
(9) after 400kg of material is fed, starting an electronic vibrator, and intermittently knocking the wall of the condenser to enable the condensed elemental arsenic to fall to the bottom of the condenser;
(10) after feeding 800kg, stopping feeding, keeping the system at a vacuum degree of 50Pa, continuously keeping the sublimation furnace and the reduction furnace at a temperature of 500 ℃ for 2h, continuously carrying out reduction and condensation, and stopping heating the sublimation furnace and the reduction furnace when the pressure of the vacuum pump system is closed and is not obviously increased;
(11) after the condenser temperature drops to below 50 ℃, begin the ejection of compact, during the ejection of compact, open the top cap of condenser earlier, then hang out the top cap of condenser with the driving, collect the back packing with the simple substance arsenic on the top cap condenser pipe and put in storage, the sample is sent the laboratory analysis, will drop condenser bottom simple substance arsenic through the discharge gate of condenser lower extreme simultaneously and take out, the sample is sent the laboratory analysis.
Reducing white arsenic by using a reducing gas, and adopting the following method:
a method of producing elemental arsenic using the apparatus for producing elemental arsenic by reduction of white arsenic described above, comprising:
(1) conveying the white arsenic to a bin of a screw feeder for standby;
(2) opening cooling water inlet and outlet valves on a condensation pipe of the condenser;
(3) pumping the vacuum of the sublimation furnace, the reduction furnace and the condenser by using a vacuum pump to ensure that the vacuum degree reaches 50 Pa;
(4) after the vacuum degree of the whole system is pumped to 50Pa, the vacuum pump is closed, reducing gas, such as hydrogen gas or carbon monoxide gas and the like, is filled into the system, and the whole pressure of the system is below 0.05 MPa;
(5) starting a heating program of the sublimation furnace and the reduction furnace, stably heating at the speed of 10 ℃/min, and stopping filling the reduction gas when the pressure is higher than 0.1 MPa;
(6) after the temperature of the sublimation furnace rises to 300 ℃ and the temperature of the reduction furnace reaches 500 ℃, starting a spiral feeder, adjusting a frequency converter to be 20Hz, feeding the sublimation furnace at a rate of 1.5 kg/min, and keeping the vacuum degree of the system at 50 Pa;
(7) keeping the temperature of the sublimation furnace at 300 ℃, the temperature of the reduction furnace at 500 ℃, and the temperature of the condenser at 50 ℃ so as to continuously sublimate, reduce and condense the materials;
(8) after 300kg of feeding, replenishing reducing gas into the reducing furnace, and ensuring that the pressure in the furnace is not higher than 0.1MPa during replenishing;
(9) after 400kg of material is fed, starting an electronic vibrator, and intermittently knocking the wall of the condenser to enable the condensed elemental arsenic to fall to the bottom of the condenser;
(10) after feeding 800kg, stopping feeding, keeping the system at a vacuum degree of 50Pa, continuously keeping the sublimation furnace and the reduction furnace at a temperature of 500 ℃ for 2h, continuously carrying out reduction and condensation, and stopping heating the sublimation furnace and the reduction furnace when the pressure of the vacuum pump system is closed and is not obviously increased;
(11) after the condenser temperature drops to below 50 ℃, begin the ejection of compact, during the ejection of compact, open the top cap of condenser earlier, then hang out the top cap of condenser with the driving, collect the back packing with the simple substance arsenic on the top cap condenser pipe and put in storage, the sample is sent the laboratory analysis, will drop condenser bottom simple substance arsenic through the discharge gate of condenser lower extreme simultaneously and take out, the sample is sent the laboratory analysis.
Example 6:
this example used the same apparatus for producing elemental arsenic by reduction of white arsenic as in example 1 and used the following method for reducing white arsenic:
white arsenic is reduced by using carbon, and the following method is adopted:
a method of producing elemental arsenic using the apparatus for producing elemental arsenic by reduction of white arsenic described above, comprising:
(1) conveying the white arsenic to a bin of a screw feeder for standby;
(2) opening cooling water inlet and outlet valves on a condensation pipe of the condenser, and adding 50kg of charcoal into the reduction furnace;
(3) pumping the vacuum of the sublimation furnace, the reduction furnace and the condenser by using a vacuum pump to ensure that the vacuum degree reaches 70 Pa;
(4) after the vacuum degree of the whole system is pumped to 70Pa, the vacuum pump is closed, and protective gas is filled into the system to ensure that the whole pressure of the system is below 0.05 MPa;
(5) starting a heating program of the sublimation furnace and the reduction furnace, and stably heating at a speed of 10 ℃/min to ensure that the overall pressure of the system is lower than 0.1 MPa;
(6) starting a spiral feeder after the temperature of the sublimation furnace rises to 300 ℃ and the temperature of the reduction furnace reaches 500 ℃, adjusting a frequency modulator to be 20Hz, and feeding the sublimation furnace at a rate of 1.5/min to keep the vacuum degree of the system at 70 Pa;
(7) keeping the temperature of the sublimation furnace at 300 ℃, the temperature of the reduction furnace at 500 ℃, and the temperature of the condenser at 50 ℃ so as to continuously sublimate, reduce and condense the materials;
(8) after 300kg of material is fed, vacuumizing a charcoal bin of a reduction furnace until the pressure reaches 70Pa, opening a charcoal bin valve, supplementing charcoal into the reduction furnace, and supplementing 50kg of charcoal once;
(9) after 400kg of material is fed, starting an electronic vibrator, and intermittently knocking the wall of the condenser to enable the condensed elemental arsenic to fall to the bottom of the condenser;
(10) after feeding 800kg, stopping feeding, keeping the system at a vacuum degree of 70Pa, continuously keeping the sublimation furnace and the reduction furnace at a temperature of 500 ℃ for 2h, continuously carrying out reduction and condensation, and stopping heating the sublimation furnace and the reduction furnace when the pressure of the vacuum pump system is closed and is not obviously increased;
(11) after the condenser temperature drops to below 50 ℃, begin the ejection of compact, during the ejection of compact, open the top cap of condenser earlier, then hang out the top cap of condenser with the driving, collect the back packing with the simple substance arsenic on the top cap condenser pipe and put in storage, the sample is sent the laboratory analysis, will drop condenser bottom simple substance arsenic through the discharge gate of condenser lower extreme simultaneously and take out, the sample is sent the laboratory analysis.
Reducing white arsenic by using a reducing gas, and adopting the following method:
a method of producing elemental arsenic using the apparatus for producing elemental arsenic by reduction of white arsenic described above, comprising:
(1) conveying the white arsenic to a bin of a screw feeder for standby;
(2) opening cooling water inlet and outlet valves on a condensation pipe of the condenser;
(3) pumping the vacuum of the sublimation furnace, the reduction furnace and the condenser by using a vacuum pump to ensure that the vacuum degree reaches 70 Pa;
(4) after the vacuum degree of the whole system is pumped to 70Pa, the vacuum pump is closed, reducing gas, such as hydrogen gas or carbon monoxide gas and the like, is filled into the system, and the whole pressure of the system is below 0.05 MPa;
(5) starting a heating program of the sublimation furnace and the reduction furnace, stably heating at the speed of 10 ℃/min, and stopping filling the reduction gas when the pressure is higher than 0.1 MPa;
(6) after the temperature of the sublimation furnace rises to 300 ℃ and the temperature of the reduction furnace reaches 500 ℃, starting a spiral feeder, adjusting a frequency converter to be 20Hz, feeding the sublimation furnace at a rate of 1.5 kg/min, and keeping the vacuum degree of the system at 70 Pa;
(7) keeping the temperature of the sublimation furnace at 300 ℃, the temperature of the reduction furnace at 500 ℃, and the temperature of the condenser at 50 ℃ so as to continuously sublimate, reduce and condense the materials;
(8) after 300kg of feeding, replenishing reducing gas into the reducing furnace, and ensuring that the pressure in the furnace is not higher than 0.1MPa during replenishing;
(9) after 400kg of material is fed, starting an electronic vibrator, and intermittently knocking the wall of the condenser to enable the condensed elemental arsenic to fall to the bottom of the condenser;
(10) after feeding 800kg, stopping feeding, keeping the system at a vacuum degree of 70Pa, continuously keeping the sublimation furnace and the reduction furnace at a temperature of 500 ℃ for 2h, continuously carrying out reduction and condensation, and stopping heating the sublimation furnace and the reduction furnace when the pressure of the vacuum pump system is closed and is not obviously increased;
(11) after the condenser temperature drops to below 50 ℃, begin the ejection of compact, during the ejection of compact, open the top cap of condenser earlier, then hang out the top cap of condenser with the driving, collect the back packing with the simple substance arsenic on the top cap condenser pipe and put in storage, the sample is sent the laboratory analysis, will drop condenser bottom simple substance arsenic through the discharge gate of condenser lower extreme simultaneously and take out, the sample is sent the laboratory analysis.
Example 7:
this example used the same apparatus for producing elemental arsenic by reduction of white arsenic as in example 1 and used the following method for reducing white arsenic:
white arsenic is reduced by using carbon, and the following method is adopted:
a method of producing elemental arsenic using the apparatus for producing elemental arsenic by reduction of white arsenic described above, comprising:
(1) conveying the white arsenic to a bin of a screw feeder for standby;
(2) opening cooling water inlet and outlet valves on a condensation pipe of the condenser, and adding 50kg of charcoal into the reduction furnace;
(3) pumping the vacuum of the sublimation furnace, the reduction furnace and the condenser by using a vacuum pump to ensure that the vacuum degree reaches 100 Pa;
(4) after the vacuum degree of the whole system is pumped to 100Pa, the vacuum pump is closed, and protective gas is filled into the system to ensure that the whole pressure of the system is below 0.05 MPa;
(5) starting a heating program of the sublimation furnace and the reduction furnace, and stably heating at a speed of 10 ℃/min to ensure that the overall pressure of the system is lower than 0.1 MPa;
(6) starting a spiral feeder after the temperature of the sublimation furnace rises to 300 ℃ and the temperature of the reduction furnace reaches 500 ℃, adjusting a frequency converter to be 20Hz, and feeding the sublimation furnace at a speed of 1.5/min to keep the vacuum degree of the system at 100 Pa;
(7) keeping the temperature of the sublimation furnace at 300 ℃, the temperature of the reduction furnace at 500 ℃, and the temperature of the condenser at 50 ℃ so as to continuously sublimate, reduce and condense the materials;
(8) after 300kg of material is fed, vacuumizing a charcoal bin of a reduction furnace until the pressure reaches 100Pa, opening a charcoal bin valve, supplementing charcoal into the reduction furnace, and supplementing 50kg of charcoal once;
(9) after 400kg of material is fed, starting an electronic vibrator, and intermittently knocking the wall of the condenser to enable the condensed elemental arsenic to fall to the bottom of the condenser;
(10) after feeding 800kg, stopping feeding, keeping the system at a vacuum degree of 100Pa, continuously keeping the sublimation furnace and the reduction furnace at a temperature of 500 ℃ for 2h, continuously carrying out reduction and condensation, and stopping heating the sublimation furnace and the reduction furnace when the pressure of the vacuum pump system is closed and is not obviously increased;
(11) after the condenser temperature drops to below 50 ℃, begin the ejection of compact, during the ejection of compact, open the top cap of condenser earlier, then hang out the top cap of condenser with the driving, collect the back packing with the simple substance arsenic on the top cap condenser pipe and put in storage, the sample is sent the laboratory analysis, will drop condenser bottom simple substance arsenic through the discharge gate of condenser lower extreme simultaneously and take out, the sample is sent the laboratory analysis.
Reducing white arsenic by using a reducing gas, and adopting the following method:
a method of producing elemental arsenic using the apparatus for producing elemental arsenic by reduction of white arsenic described above, comprising:
(1) conveying the white arsenic to a bin of a screw feeder for standby;
(2) opening cooling water inlet and outlet valves on a condensation pipe of the condenser;
(3) pumping the vacuum of the sublimation furnace, the reduction furnace and the condenser by using a vacuum pump to ensure that the vacuum degree reaches 100 Pa;
(4) after the vacuum degree of the whole system is pumped to 100Pa, the vacuum pump is closed, reducing gas, such as hydrogen gas or carbon monoxide gas and the like, is filled into the system, and the whole pressure of the system is below 0.05 MPa;
(5) starting a heating program of the sublimation furnace and the reduction furnace, stably heating at the speed of 10 ℃/min, and stopping filling the reduction gas when the pressure is higher than 0.1 MPa;
(6) after the temperature of the sublimation furnace rises to 300 ℃ and the temperature of the reduction furnace reaches 500 ℃, starting a spiral feeder, adjusting a frequency converter to be 20Hz, and feeding the sublimation furnace at a rate of 1.5 kg/min to keep the vacuum degree of the system at 100 Pa;
(7) keeping the temperature of the sublimation furnace at 300 ℃, the temperature of the reduction furnace at 500 ℃, and the temperature of the condenser at 50 ℃ so as to continuously sublimate, reduce and condense the materials;
(8) after 300kg of feeding, replenishing reducing gas into the reducing furnace, and ensuring that the pressure in the furnace is not higher than 0.1MPa during replenishing;
(9) after 400kg of material is fed, starting an electronic vibrator, and intermittently knocking the wall of the condenser to enable the condensed elemental arsenic to fall to the bottom of the condenser;
(10) after feeding 800kg, stopping feeding, keeping the system at a vacuum degree of 100Pa, continuously keeping the sublimation furnace and the reduction furnace at a temperature of 500 ℃ for 2h, continuously carrying out reduction and condensation, and stopping heating the sublimation furnace and the reduction furnace when the pressure of the vacuum pump system is closed and is not obviously increased;
(11) after the condenser temperature drops to below 50 ℃, begin the ejection of compact, during the ejection of compact, open the top cap of condenser earlier, then hang out the top cap of condenser with the driving, collect the back packing with the simple substance arsenic on the top cap condenser pipe and put in storage, the sample is sent the laboratory analysis, will drop condenser bottom simple substance arsenic through the discharge gate of condenser lower extreme simultaneously and take out, the sample is sent the laboratory analysis.
The reduction rate/% (system pressure is basically maintained around 3000 pa) of white arsenic under different reduction modes and temperatures is shown in table 1:
TABLE 1
While the principle and embodiments of the present invention have been described in detail with reference to specific examples, the description of the embodiments is only for the purpose of facilitating understanding of the method and the core concept of the present invention, and it should be noted that, for those skilled in the art, various modifications and changes can be made without departing from the principle of the present invention, and such modifications and changes also fall within the protection scope of the appended claims.
Claims (10)
1. The equipment for producing the elemental arsenic by reducing the white arsenic is characterized by comprising a spiral feeder (10), a sublimation furnace (20), a reduction furnace (30), a condenser (40), a first dust filter (50) and a first vacuum pump (60) which are sequentially and hermetically communicated from left to right, wherein a feed inlet of the spiral feeder (10) is connected with a bin (1001), a first valve (1002) is arranged between the bin (1001) and the feed inlet of the spiral feeder (10), the reduction furnace (30) comprises a furnace body (3001), an air inlet communicated with the sublimation furnace (20) is formed in the lower portion of the furnace body (3001), an air adding hole (30021) and a feeding pipe (3004) are formed in the upper end of the furnace body (3001), the feeding pipe (3004) is communicated with a charcoal bin (3006), an air exhaust hole (30061) is formed in the charcoal bin (3006), and a second valve (3005) is arranged on the feeding pipe (3004), condenser (40) is including a jar body (4001), the lower extreme of jar body (4001) is provided with the material receiving port, be provided with the electronic shaker on jar body (4001), the upper end detachably of jar body (4001) is provided with condenser pipe (4004), condenser pipe (4004) extend to the inside of jar body (4001), be provided with cooling water import and cooling water export on condenser pipe (4004).
2. The apparatus for producing elemental arsenic by reducing white arsenic according to claim 1, wherein a partition plate (3007) is horizontally arranged at the lower part of the furnace body (3001), the partition plate (3007) divides the interior of the furnace body (3001) into an upper cavity and a lower cavity (3008), an air inlet at the lower part of the furnace body (3001) is positioned above the partition plate (3007), an ash removal port (30071) is arranged on the partition plate (3007), the ash removal port (30071) is communicated with the upper cavity and the lower cavity (3008), a grid (3001) is arranged on the ash removal port (30071), an ash removal port is arranged at the bottom of the lower cavity (3008), and a third valve (3009) is connected to the ash removal port;
the dust filter is characterized by further comprising a second vacuum pump (70) and a second dust filter (80), wherein the inlet of the second dust filter (80) is connected with the third valve (3009) through a pipeline, and the outlet of the second dust filter (80) is connected with the second vacuum pump (70).
3. The apparatus for producing elemental arsenic by reduction of white arsenic according to claim 2, wherein the partition (3007) is recessed in the middle and the ash removal port (30071) is arranged in the middle of the partition (3007).
4. The apparatus for producing elemental arsenic by reduction of white arsenic according to claim 1, wherein an upper cover (3002) is detachably provided at the upper end of the furnace body (3001), a sealing strip is provided at the joint of the furnace body (3001) and the upper cover (3002), the feeding pipe is provided on the upper cover (3002), and a first cooling jacket (3003) is provided on the upper cover (3002).
5. The apparatus for producing elemental arsenic by reduction of white arsenic according to claim 1, wherein the connection between the top cover (4002) and the tank (4001) is provided with a sealing strip, and the top cover (4002) is provided with a second cooling jacket (4003).
6. A method for producing elemental arsenic using the apparatus for producing elemental arsenic by reduction of white arsenic according to any one of claims 1 to 5, comprising:
(1) conveying the white arsenic to a bin of a screw feeder for standby;
(2) opening cooling water inlet and outlet valves on a condensation pipe of a condenser, and adding 50-100 kg of charcoal into a reduction furnace;
(3) pumping vacuum of the sublimation furnace, the reduction furnace and the condenser through a vacuum pump to enable the vacuum degree to reach 10-100 Pa;
(4) after the vacuum degree of the whole system is pumped to 10-100 Pa, the vacuum pump is closed, and protective gas is filled into the system to enable the whole pressure of the system to be below 0.05 MPa;
(5) starting a heating program of the sublimation furnace and the reduction furnace, and stably heating at a speed of 10-20 ℃/min to ensure that the overall pressure of the system is lower than 0.1 MPa;
(6) starting a spiral feeder after the temperature of the sublimation furnace rises to 300-600 ℃ and the temperature of the reduction furnace reaches 500-800 ℃, adjusting a frequency modulator to be 20-30 Hz, feeding the sublimation furnace at a rate of 1.5-2.5 kg/min, and keeping the vacuum degree of the system at 10-100 Pa;
(7) keeping the temperature of a sublimation furnace at 300-600 ℃, keeping the temperature of a reduction furnace at 500-800 ℃, keeping the temperature of a condenser at 50-250 ℃, and continuously sublimating, reducing and condensing the materials;
(8) after 300kg of material is fed, vacuumizing a charcoal bin of a reduction furnace, starting a charcoal bin valve when the pressure reaches 10-100 Pa, supplementing charcoal into the reduction furnace, and supplementing 50-100 kg of charcoal once;
(9) after feeding 400-500 kg, starting an electronic vibrator, and intermittently knocking the wall of the condenser to enable the condensed elemental arsenic to fall to the bottom of the condenser;
(10) after feeding 800-1000 kg, stopping feeding, keeping the system at a vacuum degree of 10-100 Pa, continuously keeping the sublimation furnace and the reduction furnace at a temperature of 500-800 ℃ for 2h, continuously carrying out reduction and condensation, and stopping heating the sublimation furnace and the reduction furnace when the pressure of the vacuum pump system is closed and is not obviously increased;
(11) after the condenser temperature drops to below 50 ℃, begin the ejection of compact, during the ejection of compact, open the top cap of condenser earlier, then hang out the top cap of condenser with the driving, collect the back packing with the simple substance arsenic on the top cap condenser pipe and put in storage, the sample is sent the laboratory analysis, will drop condenser bottom simple substance arsenic through the discharge gate of condenser lower extreme simultaneously and take out, the sample is sent the laboratory analysis.
7. The method for producing elemental arsenic by reduction of white arsenic according to claim 6, wherein in step (11), a plurality of top covers of the condenser are prepared, and when discharging, another top cover is immediately covered after the top cover of the condenser is lifted by a crane, and steps (1) to (10) are repeated.
8. The method for producing elemental arsenic by reduction of white arsenic according to claim 6, wherein in the step (11), the cap of the condenser is lifted by a crane during discharging, and the lower part of the condenser is maintained in a negative pressure state.
9. A method for producing elemental arsenic using the apparatus for producing elemental arsenic by reduction of white arsenic according to any one of claims 1 to 5, comprising:
(1) conveying the white arsenic to a bin of a screw feeder for standby;
(2) opening cooling water inlet and outlet valves on a condensation pipe of the condenser;
(3) pumping vacuum of the sublimation furnace, the reduction furnace and the condenser through a vacuum pump to enable the vacuum degree to reach 10-100 Pa;
(4) after the vacuum degree of the whole system is pumped to 10-100 Pa, the vacuum pump is closed, and reducing gas is filled into the system to enable the whole pressure of the system to be below 0.05 MPa;
(5) starting a heating program of the sublimation furnace and the reduction furnace, stably heating at a speed of 10-20 ℃/min, and stopping filling reducing gas when the pressure is higher than 0.1 MPa;
(6) starting a spiral feeder after the temperature of the sublimation furnace rises to 300-600 ℃ and the temperature of the reduction furnace reaches 500-800 ℃, adjusting a frequency modulator to be 20-30 Hz, feeding the sublimation furnace at a rate of 1.5-2.5 kg/min, and keeping the vacuum degree of the system at 10-100 Pa;
(7) keeping the temperature of a sublimation furnace at 300-600 ℃, keeping the temperature of a reduction furnace at 500-800 ℃, keeping the temperature of a condenser at 50-250 ℃, and continuously sublimating, reducing and condensing the materials;
(8) after 300kg of feeding, replenishing reducing gas into the reducing furnace, and ensuring that the pressure in the furnace is not higher than 0.1MPa during replenishing;
(9) after feeding 400-500 kg, starting an electronic vibrator, and intermittently knocking the wall of the condenser to enable the condensed elemental arsenic to fall to the bottom of the condenser;
(10) after feeding 800-1000 kg, stopping feeding, keeping the system at a vacuum degree of 10-100 Pa, continuously keeping the sublimation furnace and the reduction furnace at a temperature of 500-800 ℃ for 2h, continuously carrying out reduction and condensation, and stopping heating the sublimation furnace and the reduction furnace when the pressure of the vacuum pump system is closed and is not obviously increased;
(11) after the condenser temperature drops to below 50 ℃, begin the ejection of compact, during the ejection of compact, open the top cap of condenser earlier, then hang out the top cap of condenser with the driving, collect the back packing with the simple substance arsenic on the top cap condenser pipe and put in storage, the sample is sent the laboratory analysis, will drop condenser bottom simple substance arsenic through the discharge gate of condenser lower extreme simultaneously and take out, the sample is sent the laboratory analysis.
10. The method for producing elemental arsenic by reduction of white arsenic according to claim 8, wherein in step (11), a plurality of top covers of the condenser are prepared, and when discharging, another top cover is immediately covered after the top cover of the condenser is lifted by a crane, and steps (1) to (10) are repeated.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113199031A (en) * | 2021-04-30 | 2021-08-03 | 广东长信精密设备有限公司 | Production method of oxygen-free high-purity cadmium powder |
| CN113481385A (en) * | 2021-07-13 | 2021-10-08 | 广西凯玺有色金属有限公司 | Process method for cleaning and refining arsenic product |
| CN114344933A (en) * | 2022-02-18 | 2022-04-15 | 郑州德凯科技有限公司 | Production device and method for preparing arsenic trioxide from crude arsenic |
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2020
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113199031A (en) * | 2021-04-30 | 2021-08-03 | 广东长信精密设备有限公司 | Production method of oxygen-free high-purity cadmium powder |
| CN113481385A (en) * | 2021-07-13 | 2021-10-08 | 广西凯玺有色金属有限公司 | Process method for cleaning and refining arsenic product |
| CN114344933A (en) * | 2022-02-18 | 2022-04-15 | 郑州德凯科技有限公司 | Production device and method for preparing arsenic trioxide from crude arsenic |
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