CN108211623B - Method and device for gas dry purification of yellow phosphorus furnace by microwave-assisted heating - Google Patents
Method and device for gas dry purification of yellow phosphorus furnace by microwave-assisted heating Download PDFInfo
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- CN108211623B CN108211623B CN201810058080.4A CN201810058080A CN108211623B CN 108211623 B CN108211623 B CN 108211623B CN 201810058080 A CN201810058080 A CN 201810058080A CN 108211623 B CN108211623 B CN 108211623B
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D50/00—Combinations of methods or devices for separating particles from gases or vapours
- B01D50/20—Combinations of devices covered by groups B01D45/00 and B01D46/00
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D51/00—Auxiliary pretreatment of gases or vapours to be cleaned
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/002—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by condensation
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/02—Preparation of phosphorus
- C01B25/027—Preparation of phosphorus of yellow phosphorus
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Abstract
The invention discloses a method and a device for dry purification of gas of a microwave-assisted heating yellow phosphorus furnace, which comprises the steps of heating yellow phosphorus furnace gas by a microwave heater, heating the furnace gas, then separating and dedusting the furnace gas in a cyclone separator to remove dust with the particle size of more than 10 microns, then feeding the furnace gas into a microwave-assisted heating membrane filter to remove dust with the particle size of 1-10 microns, and feeding the furnace gas subjected to dry dedusting into a subsequent condensation system to realize condensation of yellow phosphorus to prepare a yellow phosphorus finished product. The invention effectively solves the problem of dewing and blocking of the yellow phosphorus furnace gas of the dry dedusting system, and solves the problems of safety, environmental protection and cost puzzling the recovery of floating phosphorus and mud phosphorus in the yellow phosphorus production process. The method has the advantages of high heating rate, high efficiency and long operation period, the yield of the primary phosphorus is improved by 5-8% in the traditional process, the production labor intensity of operators is reduced, the production cost of the yellow phosphorus is reduced, and the economic benefit and the environmental protection benefit are remarkable.
Description
Technical Field
The invention relates to a method and a device for gas dry purification of a microwave-assisted heating yellow phosphorus furnace, belonging to the field of energy conservation and emission reduction of yellow phosphorus production.
Background
China is a large yellow phosphorus producing country, the total yellow phosphorus production amount is the first world, but the current yellow phosphorus industry is still a high-energy-consumption and high-pollution industry. The main method for producing yellow phosphorus by an industrial electric furnace method is to weigh qualified massive phosphorite, coke and silica and then send the weighed materials to a yellow phosphorus electric furnace bin; the mixed furnace charge enters a yellow phosphorus electric furnace through a blanking pipe, a reduction reaction is carried out under the action of electric heat, the generated furnace gas enters a three-stage or four-stage condensing tower for spray cooling to prepare crude phosphorus, and then the crude phosphorus is subjected to multi-stage refining, repeated cooking, rinsing, filtering, settling, condensation and impurity removal to obtain a yellow phosphorus product. Because the furnace gas at the outlet of the yellow phosphorus electric furnace contains a large amount of dust which enters a crude phosphorus product together with yellow phosphorus in the yellow phosphorus condensation process, and the crude phosphorus generates a large amount of sewage and sludge phosphorus in the refining process, serious environmental pollution and high treatment cost are caused. If the recovery of the phosphorus sludge is generally carried out by adopting a boiler-rotating method, namely yellow phosphorus tail gas is combusted and heated outside a boiler, firstly, about 60-70% of water in the phosphorus sludge is evaporated, then, the temperature of a hearth is gradually increased to 700-800 ℃ for phosphorus evaporation, so that the phosphorus content of residues is reduced to below 1%, and the operation period of phosphorus evaporation in each boiler is generally 6-8 hours; the method has long time consumption, high energy consumption and serious environmental pollution during combustion and slag discharge, and is a key core technology to be solved urgently in yellow phosphorus production.
In order to solve the problem that dust is brought into a condensing system to produce sludge phosphorus as a byproduct, a series of research and industrial development are carried out at home and abroad, for example, a 30kt/a yellow phosphorus device is provided with an electric dust collector at the outlet of a yellow phosphorus electric furnace, but firstly, the method needs to sinter ores entering the furnace into balls, so that the cost is increased; secondly, the temperature of furnace gas entering the dust remover is required to be higher than 600 ℃; thirdly, heat preservation is carried out on all control systems by using 300-350 ℃ inert gas; the comprehensive cost of each ton of yellow phosphorus is up to 2400 yuan, and the generation of phosphorus sludge cannot be completely eradicated. CN103708432A discloses a method, equipment and a special phosphorus collecting device for recovering yellow phosphorus from furnace gas in electric furnace phosphorus production, wherein during operation, inert preheating gas is firstly introduced to heat a filter to avoid the dewing of the phosphorus furnace gas, and the blocking of a membrane in the production process is inevitable; CN205442645U discloses a heat preservation system of yellow phosphorus furnace gas dry-method dust removal equipment, which adopts the burning yellow phosphorus tail gas to indirectly supply to the dust removal equipment so as to ensure that the phosphorus furnace gas is above the yellow phosphorus dew point, and has large energy consumption and poor heat transfer efficiency; CN105056641A discloses a 'yellow phosphorus furnace gas filtering method', which adopts a shutdown replacement mode, and introduces oxygen-containing gas to burn yellow phosphorus attached to the surface of a filter membrane, thereby ensuring the normal operation of a filtering device. These do not completely solve the problem of furnace gas condensation and condensation during the dry filtration process of yellow phosphorus furnace gas.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a method and a device for dry purification of yellow phosphorus furnace gas by microwave-assisted heating, so as to solve the problems of equipment blockage caused by yellow phosphorus furnace gas condensation in a dry dedusting system, short cleaning period of a filter element in the system and the like. According to the invention, microwave heating characteristics are utilized, microwaves are used for directly heating the wave-absorbing material, and after yellow phosphorus furnace gas passes through the heated wave-absorbing material, the temperature of the yellow phosphorus furnace gas is raised to 220-250 ℃ from 130-180 ℃ at the outlet of a yellow phosphorus electric furnace, so that the temperature of the furnace gas is ensured to be higher than the dew point temperature; the membrane filter is prepared by using wave-absorbing inorganic materials, so that microwaves directly act on a filter membrane of the membrane filter to ensure that the membrane filter is not blocked; the invention effectively solves the problem that the membrane filter is blocked by the yellow phosphorus furnace gas condensation, realizes the aim of dry dedusting of the yellow phosphorus furnace gas, and has simple operation, safety and environmental protection.
The purpose of the invention is realized by the following technical scheme:
a method for purifying yellow phosphorus furnace gas in a dry method by microwave-assisted heating comprises the steps of rapidly heating furnace gas generated in a yellow phosphorus electric furnace through a microwave heater, heating the furnace gas from 130-180 ℃ to 220-250 ℃, then separating and dedusting the furnace gas in a cyclone separator, removing dust with the particle size of more than 10 microns, then feeding the furnace gas into a microwave-assisted heating membrane filter, removing dust with the particle size of 1-10 microns, and then feeding the furnace gas into a subsequent condensation system to realize condensation of yellow phosphorus to prepare a yellow phosphorus finished product.
Preferably, in the purification process, all equipment and pipelines adopt heat preservation measures to keep the temperature at 220-250 ℃.
The method uses an apparatus comprising: the device comprises a microwave heater 1, a cyclone separator 2, a microwave auxiliary heating membrane filter 3 and a dust collector 4; the inlet 101 of the microwave heater is communicated with the furnace gas outlet of the yellow phosphorus electric furnace, the outlet 102 of the microwave heater is communicated with the inlet 201 of the cyclone separator, the gas outlet 202 of the cyclone separator is communicated with the inlet 301 of the microwave auxiliary heating membrane filter, the gas outlet 302 of the microwave auxiliary heating membrane filter is communicated with the condensing system, and the dust outlet 203 of the cyclone separator and the dust outlet 303 of the microwave auxiliary heating membrane filter are both communicated with the dust collector 4;
the microwave heater 1 is characterized in that a plurality of wave absorbing plates 104 are arranged in a conventional microwave heater, and the wave absorbing plates 104 are arranged in the microwave heater 1 and between a microwave heater inlet 101 and a microwave heater outlet 102;
the microwave auxiliary heating membrane filter 3 is provided with a filtering membrane 305 inside a conventional microwave heater and a dust outlet 303 of the microwave auxiliary heating membrane filter; the filtering membrane 305 is arranged between the inlet 301 of the microwave-assisted heating membrane filter and the gas outlet 302 of the microwave-assisted heating membrane filter, and the pore diameter of the filtering membrane 305 is less than 1 μm;
both the cyclone 2 and the dust collector 4 are conventional devices.
Preferably, the wave-absorbing plate 104 and the filtering membrane 305 are made of inorganic wave-absorbing materials, which include iron-based wave-absorbing materials (such as ferrite and polycrystalline iron fiber), carbon-based wave-absorbing materials (such as graphite, acetylene black, carbon fiber and carbon nanotube), ceramic-based wave-absorbing materials (such as silicon carbide) and other conventional inorganic wave-absorbing materials.
The working process is as follows: before the yellow phosphorus electric furnace is put into operation, a microwave heater 1 is started to heat a wave absorbing plate in the microwave heater 1, the temperature of a box body is controlled to be 250-280 ℃, after yellow phosphorus furnace gas enters the microwave heater 1, the microwave heating power is adjusted according to the temperature of gas at the outlet of the microwave heater 1, and the temperature is kept to be 220-250 ℃ (because most of the yellow phosphorus furnace gas is difficult (non) wave absorbing substances (such as yellow phosphorus steam, CO and the like) and cannot absorb microwaves, the yellow phosphorus furnace gas cannot be directly heated by the microwaves, but the wave absorbing plate is arranged in the microwave heater and is used for heating the wave absorbing plate, and when the yellow phosphorus furnace gas passes through the wave absorbing plate, the wave absorbing plate transmits heat to the yellow phosphorus furnace gas to heat the yellow phosphorus furnace gas; the heated furnace gas enters a cyclone separator 2, and dust particles with the particle size of more than 10 microns are removed under the action of centrifugal force, wherein the part of particles accounts for 85-93% of the total dust amount; the furnace gas passing through the cyclone separator 2 enters a microwave auxiliary heating membrane filter 3 to further remove dust particles with the particle size of more than 1 mu m, in order to ensure that the membrane filter is not blocked by substances below the dew point, the membrane filter 3 adopts microwave auxiliary heating, a filtering membrane is made of inorganic wave-absorbing materials, microwaves act on the filtering membrane to keep the surface temperature of the membrane at 220-250 ℃, and the microwave power is adjusted according to the temperature of the membrane filter. The dust filtered by the cyclone separator 2 and the microwave-assisted heating membrane filter 3 enters a closed dust collector 4 through respective dust outlets and is discharged. The flue gas after dust removal enters a subsequent condensation system to realize the condensation of yellow phosphorus, and the prepared yellow phosphorus finished product can be directly sold. In order to save energy, heat preservation measures are required to be taken for pipelines of equipment for purifying yellow phosphorus furnace gas by a dry method, so that heat exchange between furnace gas and the outside is reduced.
Compared with the prior art, the invention has the following advantages or positive effects:
(1) realizes dry dedusting and purification, and cancels a phosphorus bleaching and sludge recovery device. The technology of the invention is applied to realize the separation of phosphorus steam and dust before entering a condensation process, and no sludge phosphorus is generated in the subsequent process, thereby eliminating the pollution caused by the recovery of the phosphorus bleaching and the sludge phosphorus, reducing the production cost of the yellow phosphorus, and saving hot water (or steam) for the phosphorus bleaching and the phosphorus furnace tail gas for the recovery of the sludge phosphorus;
(2) the operation is simple. The microwave absorbing material is directly heated by microwaves, so that the microwave absorbing material is safe and reliable and has short flow;
(3) solves the problem of blockage caused by condensation and dewing of the yellow phosphorus furnace gas. Through two-stage control, firstly, microwave is absorbed by utilizing the characteristics of the wave-absorbing material, and the furnace gas coming out of the yellow phosphorus electric furnace is heated to 220-250 ℃ from 130-180 ℃ directly through the heated wave-absorbing material, so that condensation and dewing are avoided; secondly, the microwave is directly acted on the surface of the filter membrane, so that the problems of dewing and blockage of the filter membrane are thoroughly solved;
(4) two-stage dust removal is adopted, and the dust removal efficiency is improved. The invention adopts a combination mode of a cyclone separator and a membrane filter, firstly, dust particles larger than 10 mu m are removed by the cyclone separator, and then, tiny particles with the particle size of 1-10 mu m are removed by the membrane filter;
(5) compared with the traditional process, the yield of the primary phosphorus is improved by 5-8%, the production labor intensity of operators is reduced, and the safety of the system is improved.
Drawings
FIG. 1 is a schematic view of the apparatus according to the present invention;
FIG. 2 is a schematic longitudinal sectional view of the microwave applicator 1;
FIG. 3 is a schematic cross-sectional view of the microwave heater 1;
FIG. 4 is a schematic longitudinal sectional view of the microwave-assisted heating membrane filter 3;
FIG. 5 is a schematic cross-sectional view of the microwave-assisted heating membrane filter 3;
in the figure: 1-a microwave heater, 2-a cyclone separator, 3-a microwave auxiliary heating membrane filter, 4-a dust collector, 101-a microwave heater inlet, 102-a microwave heater outlet, 103-a microwave heater shell, 104-a wave absorption plate, 105-a microwave heater microwave break port, 201-a cyclone separator inlet, 202-a cyclone separator gas outlet, 203-a cyclone separator dust outlet, 301-a microwave auxiliary heating membrane filter inlet, 302-a microwave auxiliary heating membrane filter gas outlet, 303-a microwave auxiliary heating membrane filter dust outlet, 304-a microwave auxiliary heating membrane filter shell, 305-a filter membrane, 306-a microwave auxiliary heating membrane filter microwave break port.
Detailed Description
In order to make the objects and technical means of the present invention clearer and clearer, the present invention will be described in further detail below. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A method for dry purification of yellow phosphorus furnace gas by microwave-assisted heating comprises the following steps: heating yellow phosphorus furnace gas from 130-180 ℃ to 220-250 ℃ by adopting a microwave heater, feeding the yellow phosphorus furnace gas into a cyclone separator to remove dust particles with the particle size of more than 10 microns, feeding the furnace gas subjected to preliminary dust removal into a microwave auxiliary heating membrane filter to further remove micro particles with the particle size of 1-10 microns, discharging dust collected by the cyclone separator and the microwave auxiliary heating membrane filter to a dust collector, and feeding the purified furnace gas into a yellow phosphorus condensation absorption working section to prepare a yellow phosphorus finished product.
Example 2
The embodiment refers to embodiment 1, except that in the purifying process, all the equipment and pipelines adopt heat preservation measures to keep the temperature at 220-250 ℃.
Example 3
As shown in fig. 1 to 5, a device for a method for dry purification of yellow phosphorus furnace gas by microwave-assisted heating comprises: the device comprises a microwave heater 1, a cyclone separator 2, a microwave auxiliary heating membrane filter 3 and a dust collector 4; the inlet 101 of the microwave heater is communicated with the furnace gas outlet of the yellow phosphorus electric furnace, the outlet 102 of the microwave heater is communicated with the inlet 201 of the cyclone separator, the gas outlet 202 of the cyclone separator is communicated with the inlet 301 of the microwave auxiliary heating membrane filter, the gas outlet 302 of the microwave auxiliary heating membrane filter is communicated with the subsequent condensing system, and the dust outlet 203 of the cyclone separator and the dust outlet 303 of the microwave auxiliary heating membrane filter are both communicated with the dust collector 4.
The microwave heater 1 is characterized in that a plurality of wave absorbing plates 104 are arranged in a conventional microwave heater, and the structural components comprise a microwave heater inlet 101, a microwave heater outlet 102, a microwave heater shell 103, wave absorbing plates 104 and a microwave break opening 105 of the microwave heater; the microwave heater inlet 101 is arranged at the top of the microwave heater shell 103, the microwave heater outlet 102 is arranged at the bottom of the microwave heater shell 103, the wave absorbing plate 104 is arranged in the microwave heater 1, and the microwave break 105 of the microwave heater is uniformly arranged around the microwave heater shell 103 between the microwave heater inlet 101 and the microwave heater outlet 102 and is used for being connected with an external microwave generator; the wave absorbing plate 104 is a plate made of a ferrous wave absorbing material (ferrite).
The microwave auxiliary heating membrane filter 3 is characterized in that a filtering membrane 305 is arranged in a conventional microwave heater, and a microwave auxiliary heating membrane filter dust outlet 303 is arranged in the conventional microwave heater, and the structural components comprise a microwave auxiliary heating membrane filter inlet 301, a microwave auxiliary heating membrane filter gas outlet 302, a microwave auxiliary heating membrane filter dust outlet 303, a microwave auxiliary heating membrane filter shell 304, a filtering membrane 305 and a microwave auxiliary heating membrane filter microwave breach 306; an inlet 301 of a microwave auxiliary heating membrane filter is arranged on one side of the lower part of a shell 304 of the microwave auxiliary heating membrane filter, an air outlet 302 of the microwave auxiliary heating membrane filter is arranged on the top of the shell 304 of the microwave auxiliary heating membrane filter, a dust outlet 303 of the microwave auxiliary heating membrane filter is arranged at the bottom of the shell 304 of the microwave auxiliary heating membrane filter, a filter membrane 305 is arranged between the inlet 301 of the microwave auxiliary heating membrane filter and the air outlet 302 of the microwave auxiliary heating membrane filter, and microwave break mouths 306 of the microwave auxiliary heating membrane filter are uniformly arranged around the shell 304 of the microwave auxiliary heating membrane filter and are used for being connected with an external microwave generator; the aperture of the filter membrane 305 is smaller than 1 μm, and the filter membrane 305 is made of a ceramic-based wave-absorbing material (silicon carbide).
Both the cyclone 2 and the dust collector 4 are conventional devices.
Example 4
The present embodiment refers to embodiment 3, except that the wave absorbing plate 104 is made of an iron-based wave absorbing material (polycrystalline iron fiber); the filter membrane 305 is provided in a tubular shape, as shown in fig. 4 and 5, and is made of a carbon-based wave-absorbing material (carbon fiber).
Example 5
This example refers to example 3, except that the dust collector 4 used in this example is a screw dust discharger; the wave absorbing plate 104 is made of carbon-based wave absorbing material (graphite); the filter membrane 305 is made of a carbon-based wave-absorbing material (carbon nanotube).
Claims (1)
1. A method for dry purification of yellow phosphorus furnace gas by microwave-assisted heating comprises the steps of heating furnace gas generated in a yellow phosphorus electric furnace through a microwave heater, enabling the furnace gas to enter a cyclone separator for separation and dust removal after the temperature of the furnace gas is raised, removing dust with the particle size of more than 10 microns, then entering a microwave-assisted heating membrane filter for removing dust with the particle size of 1-10 microns, and then entering a subsequent condensation system for realizing condensation of yellow phosphorus to prepare a yellow phosphorus finished product;
the device used by the method comprises: the device comprises a microwave heater (1), a cyclone separator (2), a microwave auxiliary heating membrane filter (3) and a dust collector (4); an inlet (101) of the microwave heater is communicated with a furnace gas outlet of the yellow phosphorus electric furnace, an outlet (102) of the microwave heater is communicated with an inlet (201) of a cyclone separator, a gas outlet (202) of the cyclone separator is communicated with an inlet (301) of a microwave auxiliary heating membrane filter, a gas outlet (302) of the microwave auxiliary heating membrane filter is communicated with a condensing system, and a dust outlet (203) of the cyclone separator and a dust outlet (303) of the microwave auxiliary heating membrane filter are both communicated with a dust collector (4);
a plurality of wave absorbing plates (104) are arranged in the microwave heater (1), and the wave absorbing plates (104) are arranged in the microwave heater (1) and between the microwave heater inlet (101) and the microwave heater outlet (102);
a filtering membrane (305) is arranged in the microwave auxiliary heating membrane filter (3), and a dust outlet (303) of the microwave auxiliary heating membrane filter is arranged; the filtering membrane (305) is arranged between an inlet (301) of the microwave auxiliary heating membrane filter and a gas outlet (302) of the microwave auxiliary heating membrane filter, and a dust outlet (303) of the microwave auxiliary heating membrane filter is arranged at the bottom of the microwave auxiliary heating membrane filter (3);
heating the furnace gas to 220-250 ℃ through a microwave heater;
in the purification process, all equipment and pipelines adopt heat preservation measures to keep the temperature at 220-250 ℃;
the wave absorbing plate (104) and the filtering membrane (305) are made of inorganic wave absorbing materials; the inorganic wave-absorbing material is ferrite, polycrystalline iron fiber, graphite, acetylene black, carbon fiber, carbon nano tube or silicon carbide;
the pore size of the filter membrane (305) is less than 1 μm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810058080.4A CN108211623B (en) | 2018-01-22 | 2018-01-22 | Method and device for gas dry purification of yellow phosphorus furnace by microwave-assisted heating |
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| CN201810058080.4A CN108211623B (en) | 2018-01-22 | 2018-01-22 | Method and device for gas dry purification of yellow phosphorus furnace by microwave-assisted heating |
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| CN108211623B true CN108211623B (en) | 2020-10-27 |
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| CN109078959A (en) * | 2018-08-09 | 2018-12-25 | 南京三乐微波技术发展有限公司 | A kind of Biohazard Waste microwave heating appts and its processing method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5453116A (en) * | 1994-06-13 | 1995-09-26 | Minnesota Mining And Manufacturing Company | Self supporting hot gas filter assembly |
| CN1963334A (en) * | 2006-11-30 | 2007-05-16 | 长沙隆泰微波热工有限公司 | A gas heating apparatus by microwave |
| CN103508429A (en) * | 2013-09-29 | 2014-01-15 | 成都易态科技有限公司 | Yellow phosphorus preparation method and yellow phosphorus preparation equipment |
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- 2018-01-22 CN CN201810058080.4A patent/CN108211623B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5453116A (en) * | 1994-06-13 | 1995-09-26 | Minnesota Mining And Manufacturing Company | Self supporting hot gas filter assembly |
| CN1963334A (en) * | 2006-11-30 | 2007-05-16 | 长沙隆泰微波热工有限公司 | A gas heating apparatus by microwave |
| CN103508429A (en) * | 2013-09-29 | 2014-01-15 | 成都易态科技有限公司 | Yellow phosphorus preparation method and yellow phosphorus preparation equipment |
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