CN108439358B - Device and process for producing yellow phosphorus by microwave method - Google Patents
Device and process for producing yellow phosphorus by microwave method Download PDFInfo
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- CN108439358B CN108439358B CN201810294521.0A CN201810294521A CN108439358B CN 108439358 B CN108439358 B CN 108439358B CN 201810294521 A CN201810294521 A CN 201810294521A CN 108439358 B CN108439358 B CN 108439358B
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- C01B25/00—Phosphorus; Compounds thereof
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- C01B25/047—Purification of phosphorus of yellow phosphorus
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Abstract
The invention relates to a device for producing yellow phosphorus by a microwave method and a production process thereof, belonging to the technical field of yellow phosphorus preparation, wherein the device comprises a tank body, a first microwave feed-in component and a second microwave feed-in component, wherein the first microwave feed-in component is positioned at the top of the tank body and comprises a plurality of feed-in waveguides and a plurality of microwave reflecting sheets, the microwaves are fed into the tank body and are focused on a reduction reaction zone, meanwhile, the interference between the feed-in waveguides when the microwaves are fed in from the top of the tank body is eliminated by the aid of the microwave reflecting sheets, the second microwave feed-in component is positioned at the bottom of the tank body and is provided with a plurality of dielectric waveguides, and aluminum oxide ceramics are adopted as the dielectric waveguides to feed the microwaves from the bottom of the tank body to the reduction reaction zone so as to overcome the influence of strong microwave absorption materials on the microwaves, so as to maintain the continuous microwave chemical reaction of the reduction reaction zone, thereby achieving the environmental conditions required by yellow phosphorus production, and the characteristics of low energy consumption and low corrosion, and the maintenance cost of the tank body.
Description
Technical Field
The invention belongs to the technical field of yellow phosphorus preparation, and particularly relates to a device and a production process for producing yellow phosphorus by a microwave method.
Background
The world phosphorus production history is nearly 1 century, the development of the phosphorus industry has undergone a small to large development history, the single electric furnace capacity of the traditional yellow phosphorus electric furnace is developed from 200kVA to the single electric furnace capacity of today, 4.5-6 kVA, and the power consumption of the phosphorus industry is the first of the chemical industry.
At present, china has developed into a world yellow phosphorus large country, and the productivity is over 120 ten thousand tons/year. Elemental phosphorus is a vital element of human life, and phosphorus is also important in industry, such as computer manufacturing, automobiles, metallurgy, medicine, dye and the like, but is not separated from elemental phosphorus, so that the phosphorus industry is one of the most important basic industries in the industry of China, but yellow phosphorus production pollution is serious. In order to meet the trend of grabbing the machine to shake the yellow phosphorus production industry in China, in the current society of resource shortage, energy shortage and increasingly aggravated environmental pollution, how to solve the problems of high energy consumption and high pollution existing in the traditional phosphorus production process is a urgent need to be solved.
Disclosure of Invention
In order to solve the problems, the inventor utilizes the microwave characteristic of the yellow phosphorus preparation raw material to produce yellow phosphorus by microwaves to form a new process and a new device for preparing yellow phosphorus, which are different from an electric furnace method, so as to solve the problems of high energy consumption and high pollution in the traditional process.
In order to achieve the above purpose, the present invention provides the following technical solutions:
an apparatus for producing yellow phosphorus by a microwave method, comprising:
the device comprises a tank body, wherein the top of the tank body is provided with a feed inlet for throwing in preparation raw materials and an air outlet for discharging yellow phosphorus steam, the bottom of the tank body is provided with a discharge outlet for discharging waste residues, the inner cavity of the tank body is set to be in a micro-positive pressure state, and the side wall of the tank body is divided into an outer wall, an inner wall and a vacuum heat preservation layer positioned between the outer wall and the inner wall;
the first microwave feed-in component is used for feeding microwaves into the tank body and is positioned at the top of the tank body, and comprises a plurality of feed-in waveguides and a plurality of microwave reflecting sheets, wherein the feed-in waveguides are arranged along the horizontal direction, the tail ends of the feed-in waveguides penetrate through the side wall of the tank body and extend to the inner cavity of the tank body, and the microwave reflecting sheets are of an inclined structure and are connected with the tail ends of the feed-in waveguides;
the second microwave feed-in component is positioned at the bottom of the tank body, the second microwave feed-in component is a plurality of dielectric waveguides, the dielectric waveguides are arranged along the vertical direction, and the top ends of the dielectric waveguides penetrate through the bottom surface of the tank body and extend to the inner cavity of the tank body;
the preparation raw materials put in through the feed inlet are piled up in the inner cavity to form a raw material zone, the preparation raw materials in the raw material zone react under the action of microwaves to form a reduction reaction zone, the preparation raw materials react in the reduction reaction zone to form a waste residue zone, microwaves fed in through the feed-in waveguide are reflected and focused to the reduction reaction zone through the microwave reflecting sheet, the top end of the dielectric waveguide extends to the reduction reaction zone, and the discharge port is communicated with the waste residue zone.
Further, the feed-in waveguides and the microwave reflecting sheets are the same in number, and the feed-in waveguides are uniformly distributed along the height of the tank body and the circumferential direction of the tank body.
Further, the plurality of dielectric waveguides are positioned on different circumferences of the bottom surface of the tank body, and the plurality of dielectric waveguides positioned on the same circumference are uniformly distributed.
Further, the microwave reflecting sheet is made of total reflection microwave material, and the included angle between the microwave reflecting sheet and the horizontal plane is 35-45 degrees.
Further, among the plurality of microwave reflecting sheets adjacent in the vertical direction, the included angle between the microwave reflecting sheet located at the high position and the horizontal plane is smaller than the included angle between the microwave reflecting sheet located at the low position and the horizontal plane.
Further, the dielectric waveguide is made of aluminum oxide ceramic.
Further, the temperature of the reduction reaction zone is 1300 ℃ to 1500 ℃, and the temperature of the raw material zone is not higher than 600 ℃.
Further, temperature sensors are arranged on the side wall of the tank body corresponding to the raw material area, the reduction reaction area and the waste residue area, and are in communication connection with the control unit.
In addition, the invention also provides a production process of the device for producing yellow phosphorus by the microwave method, which comprises the following steps:
s1: feeding a preparation raw material into the inner cavity through a feed inlet;
s2: feeding microwaves into the inner cavity through the feed-in waveguide and the dielectric waveguide, adjusting microwave power, ensuring that the temperature of the reduction reaction zone is controlled to 1300-1500 ℃, and simultaneously, ensuring that the temperature of the raw material zone is not higher than 600 ℃;
s3: and (3) discharging yellow phosphorus steam from the air outlet, and then, feeding the yellow phosphorus steam into a water cooling system, further, recovering yellow phosphorus, and discharging waste residues generated by the reaction from the discharge outlet in a molten state.
Further, in the step S1, the preparation raw materials include silica and coking coal, wherein the weight of the coking coal accounts for 8% -12% of the total weight of the preparation raw materials.
The beneficial effects of the invention are as follows:
1. the microwave characteristics of the preparation raw materials and a special microwave feed-in mode are utilized to establish and realize a stable environment required by yellow phosphorus production, the interference between feed-in waveguides is eliminated by means of the microwave reflector plate when microwaves are fed in from the top of the tank body, meanwhile, aluminum oxide ceramics are adopted as dielectric waveguides to feed the microwaves into the reduction reaction zone from the bottom of the tank body, so that the influence of strong microwave absorption materials on the microwaves is overcome, the continuous microwave chemical reaction of the reduction reaction zone is maintained, the environment condition required by yellow phosphorus production is achieved, the characteristics of low energy consumption and low corrosion are achieved, and the maintenance cost of the tank body is reduced.
2. The preparation raw materials do not relate to the consumption of graphite and the up-and-down movement of a graphite electrode, thereby being beneficial to reducing the production cost of yellow phosphorus, eliminating the gas escape in the production process and the influence of the gas escape on the environment, and being safe and environment-friendly.
Drawings
FIG. 1 is a schematic view of the overall structure of the present invention;
fig. 2 is a schematic view of the partial structure at a in fig. 1.
In the accompanying drawings: 1-tank body, 2-feed inlet, 3-gas outlet, 4-discharge outlet, 5-raw material zone, 6-reduction reaction zone, 7-waste residue zone, 8-first microwave feed-in component, 9-second microwave feed-in component, 10-microwave, 11-microwave, 12-feed-in waveguide, 13-microwave reflector plate, 14-inner cavity and 15-vacuum heat preservation layer.
Wherein, the arrows in fig. 1-2 represent the feeding direction of microwaves, and the inner region of the dashed line frame in fig. 1 represents the reduction reaction zone.
Detailed Description
In order to make the technical solution of the present invention better understood by those skilled in the art, the technical solution of the present invention will be clearly and completely described below with reference to the accompanying drawings, and based on the embodiments in the present application, other similar embodiments obtained by those skilled in the art without making creative efforts should fall within the scope of protection of the present application. In addition, directional words such as "upper", "lower", "left", "right", and the like, as used in the following embodiments are merely directions with reference to the drawings, and thus, the directional words used are intended to illustrate, not to limit, the invention.
Embodiment one:
as shown in fig. 1-2, an apparatus for producing yellow phosphorus by a microwave method comprises a tank 1, a first microwave feed-in assembly 8 and a second microwave feed-in assembly 9. The top of the tank body 1 is provided with a feed inlet 2 for throwing in preparation raw materials and an air outlet 3 for discharging yellow phosphorus steam, the bottom of the tank body is provided with a discharge outlet 4 for discharging waste residues, an inner cavity 14 of the tank body is set to be in a micro-positive pressure state, and meanwhile, the side wall of the tank body 1 is divided into an outer wall, an inner wall and a vacuum heat insulation layer 15 positioned between the outer wall and the inner wall, that is, the inner cavity 14 is in a closed micro-positive pressure state. The inner cavity 14 is used for containing preparation raw materials and providing a reaction space for the preparation raw materials, the first microwave feeding assembly 8 is used for feeding microwaves 11 to the inner cavity 14, and the second microwave feeding assembly 9 is used for feeding microwaves 10 to the inner cavity 14.
The raw materials for preparation comprise silica and coking coal, the raw materials for preparation are piled up in the inner cavity 14 to form a raw material zone 5, when the temperature is lower than 600 ℃, the silica is a weak microwave absorbing substance, when the temperature is higher than 600 ℃, the silica is a strong microwave absorbing substance, and the microwave absorbing property of the coking coal is stable and is a strong microwave absorbing substance. Therefore, in order to ensure that the raw material for production located in the raw material zone 5 has a good wave-transmitting property, it is necessary to ensure that the weight of the coking coal is strictly 8% -12% of the total weight of the raw material, and that the temperature of the raw material zone 5 is not higher than 600 ℃. The microwaves 10 and 11 fed into the cavity 14 promote the local temperature inside the preparation raw material (namely, 10cm-50cm below the surface of the raw material zone 5) to exceed 600 ℃, the silica is converted into a strong microwave absorbing substance in the zone, and the local temperature in the zone is further promoted to rapidly rise to the yellow phosphorus reduction reaction temperature, namely 1300-1500 ℃, at the moment, the silica and the coking coal undergo oxidation-reduction reaction under the microwave condition to form a reduction reaction zone 6, the preparation raw material forms a waste residue zone 7 after the reduction reaction zone 6 is reacted, and the discharge port 4 is communicated with the waste residue zone 7. Thus, in order to maintain a stable production environment, the reduction reaction zone 6 temperature is 1300 ℃ to 1500 ℃. The critical temperature of the microwave chemical reaction is lower than that of the traditional process due to the non-thermal effect of the microwave chemical reaction, and the chemical reaction speed is higher than that of the traditional process, so that the yellow phosphorus production energy consumption is lower than that of the traditional process, in addition, the traditional process has very strict corrosiveness under the condition of the traditional process due to the fact that the local temperature is required to exceed 2000 ℃ and an arc (the temperature of an arc zone exceeds 3000 ℃), and the reaction temperature is controlled to 1300-1500 ℃, so that the corrosion of the chemical reaction to the tank body 1 is obviously reduced, and the maintenance cost of the tank body is reduced.
The first microwave feed-in component 8 is located at the top of the tank 1, and comprises a plurality of feed-in waveguides 12 and a plurality of microwave reflecting sheets 13, where the feed-in waveguides 12 are disposed along a horizontal direction, and the ends of the feed-in waveguides extend through the side wall of the tank 1 (i.e. sequentially penetrate through the outer wall, the vacuum insulation layer 15 and the inner wall) and extend to the inner cavity 14 of the tank, and the microwave reflecting sheets 13 are in an inclined structure and are connected with the ends of the feed-in waveguides 12, and meanwhile, microwaves 11 fed in through the feed-in waveguides 12 are reflected and focused to the reduction reaction zone 6 by the microwave reflecting sheets 12. That is, the microwaves 11 horizontally enter the tank 1, and the microwaves 11 are converted from horizontal radiation to downward radiation and radiated to the reduction reaction zone 6 by the microwave reflecting sheet 13.
The feed-in waveguides 12 and the microwave reflecting sheets 13 are the same in number, and the feed-in waveguides 12 are uniformly distributed along the height of the tank 1 and the circumferential direction of the tank. The microwave reflecting sheet 13 is made of a total reflection microwave material, the included angle between the total reflection microwave material and the horizontal plane is 35-45 degrees, and among the plurality of microwave reflecting sheets 13 adjacent to each other in the vertical direction, the included angle between the microwave reflecting sheet 13 positioned at the high position and the horizontal plane is smaller than the included angle between the microwave reflecting sheet 13 positioned at the low position and the horizontal plane, that is, the included angles between the plurality of microwave reflecting sheets 13 adjacent to each other in the vertical direction and the horizontal plane are sequentially increased from top to bottom. By fine tuning the inclination angle of the microwave reflecting plate 13, the microwaves 11 fed by the feed-in waveguides 12 are focused in the reduction reaction area 6. Meanwhile, as the radiation direction of the microwaves 11 is downward, the microwave coupling in the same horizontal plane is reduced, and the mutual interference between different feed-in waveguides 12 in the same horizontal plane is reduced, so that each feed-in waveguide 12 can continuously work at the same time. In addition, in the vertical direction, the microwave reflecting sheet 13 has an effective isolation effect on adjacent microwaves 11, so that mutual interference between adjacent feed-in waveguides 12 in the vertical direction is reduced, and each feed-in waveguide 12 can continuously work at the same time.
The second microwave feed-in assembly 9 is located at the bottom of the tank 1, and includes a plurality of dielectric waveguides, where the dielectric waveguides are disposed along a vertical direction, and the top ends of the dielectric waveguides penetrate through the bottom surface of the tank 1 and extend to the reduction reaction zone 6. Meanwhile, the dielectric waveguides are located on different circumferences of the bottom surface of the tank body 1, and the dielectric waveguides located on the same circumference are uniformly distributed. When the chemical reaction occurs in the preparation raw materials, silica is converted into a strong microwave absorbing substance, and microwaves are seriously affected to enter the reduction reaction zone 6, at this time, considering that aluminum oxide ceramic is a good wave-transmitting substance, the microwave absorbing performance of the aluminum oxide ceramic is stable in the range of 1300-1500 ℃ and the aluminum oxide ceramic does not absorb microwaves, the inventor adopts the aluminum oxide ceramic to prepare a dielectric waveguide so as to overcome the influence of the strong microwave absorbing material on the microwaves entering the chemical reaction zone, and microwaves 10 are fed into the reduction reaction zone 6 from the bottom of the tank body 1 to maintain the continuous microwave chemical reaction in the zone.
In summary, when the microwaves 11 are fed from the top of the tank 1, they are focused on the reduction reaction area 6 by means of the microwave reflecting sheet 13, and meanwhile, isolation between different feed-in waveguides 12 is achieved, so that interference between the feed-in waveguides 12 is eliminated. When microwaves 10 are fed from the bottom of the tank 1, the interference between the dielectric waveguides is eliminated by the strong microwave absorption characteristics of the prepared material in the reduction reaction zone 6. The inventor makes full use of the microwave characteristics of the preparation raw materials, establishes a special microwave feed-in mode, realizes that a plurality of microwave beams are fed into the reduction reaction zone 6 effectively and mutually without interference, and the temperature in the inner cavity 14 can be controlled in a partitioning manner, and establishes and realizes a stable environment required by yellow phosphorus production to prepare yellow phosphorus. In addition, temperature sensors which are in communication connection with the control unit are arranged on the side wall of the tank body 1 corresponding to the raw material zone 5, the reduction reaction zone 6 and the waste residue zone 7 and are used for monitoring the temperature in real time and uploading temperature signals to the control unit so as to serve as the basis for adjusting the power of the microwaves 10 and the microwaves 11 and guaranteeing the temperature required by the reaction.
Specifically, the process for preparing yellow phosphorus by using the device for producing yellow phosphorus by using the microwave method comprises the following steps:
firstly, putting silica and coking coal into an inner cavity 14 through a feed inlet 2, then feeding microwaves 11 and 10 into the inner cavity 14 through a feed-in waveguide 12 and a medium wave guide, regulating microwave power according to a temperature signal uploaded by a temperature sensor, ensuring that the temperature of a reduction reaction zone 6 is controlled at 1300-1500 ℃, simultaneously, ensuring that the temperature of a raw material zone 5 is not higher than 600 ℃, finally, discharging yellow phosphorus steam from an air outlet 3, then, entering a water cooling system, further recovering yellow phosphorus, and discharging waste residues generated by reaction from a discharge port 4 in a molten state. Compared with the traditional process, the invention does not relate to the problems of graphite consumption and up-and-down movement of the graphite electrode, reduces the production cost of yellow phosphorus, and eliminates the influence of gas escape and gas escape on the environment in the production process.
The foregoing detailed description of the invention has been presented for purposes of illustration and description, but is not intended to limit the scope of the invention, i.e., the invention is not limited to the details shown and described.
Claims (10)
1. An apparatus for producing yellow phosphorus by microwave method, comprising:
the device comprises a tank body, wherein the top of the tank body is provided with a feed inlet for throwing in preparation raw materials and an air outlet for discharging yellow phosphorus steam, the bottom of the tank body is provided with a discharge outlet for discharging waste residues, the inner cavity of the tank body is set to be in a micro-positive pressure state, and the side wall of the tank body is divided into an outer wall, an inner wall and a vacuum heat preservation layer positioned between the outer wall and the inner wall;
the first microwave feed-in component is used for feeding microwaves into the tank body and is positioned at the top of the tank body, and comprises a plurality of feed-in waveguides and a plurality of microwave reflecting sheets, wherein the feed-in waveguides are arranged along the horizontal direction, the tail ends of the feed-in waveguides penetrate through the side wall of the tank body and extend to the inner cavity of the tank body, and the microwave reflecting sheets are of an inclined structure and are connected with the tail ends of the feed-in waveguides;
the second microwave feed-in component is positioned at the bottom of the tank body, the second microwave feed-in component is a plurality of dielectric waveguides, the dielectric waveguides are arranged along the vertical direction, and the top ends of the dielectric waveguides penetrate through the bottom surface of the tank body and extend to the inner cavity of the tank body;
the preparation raw materials put in through the feed inlet are piled up in the inner cavity to form a raw material zone, the preparation raw materials in the raw material zone react under the action of microwaves to form a reduction reaction zone, the preparation raw materials react in the reduction reaction zone to form a waste residue zone, microwaves fed in through the feed-in waveguide are reflected and focused to the reduction reaction zone through the microwave reflecting sheet, the top end of the dielectric waveguide extends to the reduction reaction zone, and the discharge port is communicated with the waste residue zone.
2. The device for producing yellow phosphorus by using a microwave method according to claim 1, wherein the feed-in waveguides and the microwave reflecting sheets have the same number, and the feed-in waveguides are uniformly distributed along the height of the tank body and the circumference of the tank body.
3. The device for producing yellow phosphorus by using a microwave method according to claim 1, wherein the plurality of dielectric waveguides are positioned on different circumferences of the bottom surface of the tank body, and the plurality of dielectric waveguides positioned on the same circumference are uniformly distributed.
4. The apparatus for producing yellow phosphorus by microwave method according to claim 1, wherein the microwave reflecting sheet is made of total reflection microwave material and has an included angle of 35 ° -45 ° with respect to the horizontal plane.
5. The apparatus for producing yellow phosphorus by microwave method according to claim 4, wherein an angle between a microwave reflecting sheet located at a higher position and a horizontal plane is smaller than an angle between a microwave reflecting sheet located at a lower position and a horizontal plane among the plurality of microwave reflecting sheets adjacent in a vertical direction.
6. The apparatus for producing yellow phosphorus by microwave method according to any one of claims 1-5, wherein the dielectric waveguide is made of aluminum oxide ceramic.
7. The apparatus for producing yellow phosphorus by microwave method according to claim 6, wherein the temperature of the reduction reaction zone is 1300 ℃ to 1500 ℃ and the temperature of the raw material zone is not higher than 600 ℃.
8. The device for producing yellow phosphorus by using the microwave method according to claim 6, wherein temperature sensors are arranged on the side wall of the tank body corresponding to the raw material area, the reduction reaction area and the waste residue area, and the temperature sensors are in communication connection with the control unit.
9. A process for producing yellow phosphorus by a microwave method as claimed in any one of claims 1 to 8, comprising the steps of:
s1: feeding a preparation raw material into the inner cavity through a feed inlet;
s2: feeding microwaves into the inner cavity through the feed-in waveguide and the dielectric waveguide, adjusting microwave power, ensuring that the temperature of the reduction reaction zone is controlled to 1300-1500 ℃, and simultaneously, ensuring that the temperature of the raw material zone is not higher than 600 ℃;
s3: and (3) discharging yellow phosphorus steam from the air outlet, and then, feeding the yellow phosphorus steam into a water cooling system, further, recovering yellow phosphorus, and discharging waste residues generated by the reaction from the discharge outlet in a molten state.
10. The process according to claim 9, wherein in step S1, the preparation raw materials include silica and coking coal, wherein the coking coal accounts for 8% -12% of the total weight of the preparation raw materials.
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| US6207024B1 (en) * | 1999-10-04 | 2001-03-27 | Astaris Llc | Method of preparing phosphorus |
| CN202304314U (en) * | 2011-09-30 | 2012-07-04 | 山东博润工业技术有限公司 | Turntable-type low-rank coal microwave quality improvement equipment |
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