Process for preparing battery-grade manganese oxide and by-product sulfuric acid by roasting high-purity manganese sulfate and sulfur

文档序号:1349567 发布日期:2020-07-24 浏览:19次 中文

阅读说明:本技术 高纯硫酸锰与硫磺焙烧制备电池级氧化锰与附产硫酸工艺 (Process for preparing battery-grade manganese oxide and by-product sulfuric acid by roasting high-purity manganese sulfate and sulfur ) 是由 于金圣 于国安 张岩 于 2020-04-03 设计创作,主要内容包括:一种高纯硫酸锰与硫磺焙烧制备电池级氧化锰与附产硫酸工艺,用20%的稀硫酸洗涤低品位硅锰合金除尘灰,除渣后得到硫酸盐溶液,调节硫酸盐溶液中硫酸钙、硫酸铝、硫酸镁的浓度,以使硫酸钙、硫酸铝、硫酸镁生成钙镁矾共沉淀,然后加入一定量的锰粉,并分离钙镁矾,将得到的硫酸锰溶液高温结晶,并分离结晶物,将得到的硫酸锰干燥后,与硫磺一起在氧气气氛中燃烧,得到一氧化锰和二氧化硫,本发明方法利用废稀硫酸处理硅锰合金除尘灰,能有效回收硅锰合金除尘灰中的锰元素制取一氧化锰与附产硫酸,通过共沉淀和置换两种反应来提纯硫酸锰溶液,得到高纯硫酸锰,利用硫酸锰与硫磺一起在氧气气氛中燃烧,能直接生成一氧化锰,不必额外消耗热能。(A process for preparing battery-grade manganese oxide and by-product sulfuric acid by roasting high-purity manganese sulfate and sulfur includes washing low-grade silicomanganese alloy dust by 20% of dilute sulfuric acid, removing slag to obtain sulfate solution, regulating the concentrations of calcium sulfate, aluminum sulfate and magnesium sulfate in the sulfate solution to make calcium sulfate, aluminum sulfate and magnesium sulfate generate calcium-magnesium-alum coprecipitation, adding certain amount of manganese powder, separating calcium-magnesium-alum, high-temperature crystallizing the obtained manganese sulfate solution, separating crystal, drying the obtained manganese sulfate, burning the manganese sulfate and sulfur in oxygen atmosphere to obtain manganese monoxide and sulfur dioxide, treating the silicomanganese alloy dust by waste dilute sulfuric acid to effectively recover manganese element in the silicomanganese dust to prepare manganese monoxide and by-product sulfuric acid, purifying the manganese sulfate solution by coprecipitation and replacement to obtain high-purity manganese sulfate, manganese sulfate and sulfur are combusted in oxygen atmosphere, so that manganese monoxide can be directly generated without additional consumption of heat energy.)

1. A process for preparing battery-grade manganese oxide and by-product sulfuric acid by roasting high-purity manganese sulfate and sulfur is characterized by comprising the following steps:

the method comprises the following steps: washing low-grade silicon-manganese alloy dust removal ash by using 20% dilute sulfuric acid, and removing slag to obtain a sulfate solution, wherein the sulfate comprises manganese sulfate, calcium sulfate, aluminum sulfate and magnesium sulfate;

step two: adjusting the concentrations of calcium sulfate, aluminum sulfate and magnesium sulfate in the sulfate solution to enable the calcium sulfate, the aluminum sulfate and the magnesium sulfate to generate calcium-magnesium-alum coprecipitation, then adding a certain amount of manganese powder, and separating the calcium-magnesium-alum to obtain a manganese sulfate solution;

step three: crystallizing the manganese sulfate solution obtained in the second step at a high temperature, and separating a crystal to obtain manganese sulfate;

step four: drying the manganese sulfate obtained in the third step, and then burning the manganese sulfate and sulfur together in an oxygen atmosphere to obtain manganese monoxide and sulfur dioxide;

step five: reacting sulfur dioxide with oxygen to generate sulfur trioxide by taking vanadium pentoxide as a catalyst;

step six: the sulfur trioxide reacts with water to produce sulfuric acid.

2. The process for preparing battery-grade manganese oxide and by-product sulfuric acid by roasting high-purity manganese sulfate and sulfur according to claim 1, wherein: in the fourth step, manganese sulfate obtained in the third step is dried and then roasted together with sulfur in a silicon carbide lining roasting furnace, the silicon carbide lining roasting furnace comprises a furnace body and an air blower, the furnace body is a sealed cylinder, the furnace body comprises a shell, a rigid anticorrosive layer is coated on the inner wall of the shell, the anticorrosive layer is made of silicon carbide materials, a horizontal partition plate is arranged in the cylinder and is used for dividing the furnace body into a reaction chamber and an air equalizing chamber from top to bottom, the air blower comprises a blast pipe, one end of the blast pipe is communicated with the inner cavity of the air equalizing chamber, the other end of the blast pipe is connected with an outlet of the air blower, a plurality of air caps are arranged on the partition plate and are uniformly distributed on the partition plate, an air inlet of the air cap is communicated with the air equalizing chamber, and an air outlet of the air cap is communicated with the inner cavity of the.

3. The process for preparing battery-grade manganese oxide and by-product sulfuric acid by roasting silicon high-purity manganese sulfate and sulfur according to claim 1, wherein: in the third step, manganese sulfate solution is subjected to high-temperature crystallization in a continuous high-temperature high-pressure crystallizer, the continuous high-temperature high-pressure crystallizer comprises a pipe body, a heat exchanger, a heating part and a storage tank, the pipe body is a long and thin sealed cylinder body, the pipe body is vertically arranged, the heat exchanger is arranged in the pipe body and is close to the top wall of the pipe body, the heat exchanger divides the inner cavity of the pipe body into a buffer chamber and a crystallization chamber, the buffer section is positioned above the heat exchanger, the crystallization section is positioned below the heat exchanger, an inlet of a pipe pass of the heat exchanger is communicated with the buffer chamber, an outlet of the pipe pass of the heat exchanger is communicated with the crystallization chamber, the heating part is arranged at the lower part of the side wall of the pipe body to heat the inner cavity of the crystallization chamber, a crystallization liquid inlet is arranged at the upper part of the side wall of the pipe body, the crystallization liquid inlet, and a second mother liquid port and a third mother liquid port are arranged on the side wall of the tube body between the first mother liquid port and the crystallization liquid inlet, the first mother liquid port is connected with the second mother liquid port through a pipeline, the second mother liquid port is connected with an inlet of a shell pass of the heat exchanger, an outlet of the shell pass of the heat exchanger is connected with the third mother liquid port, and a crystallization product outlet is arranged on the bottom wall of the tube body.

4. The process for preparing battery-grade manganese oxide and by-product sulfuric acid by roasting high-purity manganese sulfate and sulfur according to claim 3, wherein: the continuous high-temperature high-pressure crystallizer further comprises a pressure pump, wherein an inlet of the pressure pump is connected with an outlet of the storage tank, and an outlet of the pressure pump is connected with a crystallization liquid inlet.

5. The process for preparing battery-grade manganese oxide and by-product sulfuric acid by roasting high-purity manganese sulfate and sulfur according to claim 3, wherein: the top wall of the pipe body is provided with a safety outlet, and the safety outlet is provided with a safety valve.

6. The process for preparing battery-grade manganese oxide and by-product sulfuric acid by roasting high-purity manganese sulfate and sulfur according to claim 4, wherein: the pressure in the tube body is 18kg/cm2The temperature of the crystalline section of the tube is 200 ℃.

7. The process for preparing battery-grade manganese oxide and by-product sulfuric acid by roasting high-purity manganese sulfate and sulfur according to claim 1, wherein: in the first step, a certain amount of iron sulfide is added in the process of washing the low-grade silicon-manganese alloy dedusting ash by using 20% dilute sulfuric acid.

8. The process for preparing battery-grade manganese oxide and by-product sulfuric acid by roasting high-purity manganese sulfate and sulfur according to claim 1, wherein: the 20% dilute sulfuric acid is prepared by sulfuric acid with different concentrations.

9. The process for preparing battery-grade manganese oxide and by-product sulfuric acid by roasting high-purity manganese sulfate and sulfur according to claim 8, wherein: and (4) returning mother liquor obtained by separating the crystal in the step three to the step one to prepare 20% dilute sulfuric acid.

10. The process for preparing battery-grade manganese oxide and by-product sulfuric acid by roasting high-purity manganese sulfate and sulfur according to claim 1, wherein: the low-grade silicon-manganese alloy dust-removing ash contains 13-17% of metal manganese.

Technical Field

The invention relates to the technical field of manganese monoxide production, in particular to a process for preparing battery-grade manganese oxide and by-product sulfuric acid by roasting high-purity manganese sulfate and sulfur.

Background

When the silicon-manganese alloy is produced, dust is generated inevitably, the dust contains oxidation state manganese, and the content of the oxidation state manganese in the dust is 13-17% calculated by the content of metal manganese. Most of enterprises in the metallurgical industry are subjected to small part of recovery, and most of the rest of enterprises are buried, so that the serious waste of manganese resources is caused, and ten-thousand-ton waste dilute sulfuric acid is generated by some of the enterprises to be treated every year. Therefore, how to produce the manganese monoxide and the sulfuric acid by-product of the battery by combining the dust and the waste dilute sulfuric acid saves the production raw material cost, solves the problem of waste dilute sulfuric acid treatment and has great significance for the development of enterprises.

Disclosure of Invention

In view of the above, it is necessary to provide a process for preparing battery-grade manganese oxide and by-product sulfuric acid by roasting high-purity manganese sulfate and sulfur.

A process for preparing battery-grade manganese oxide and by-product sulfuric acid by roasting high-purity manganese sulfate and sulfur comprises the following steps:

the method comprises the following steps: washing low-grade silicon-manganese alloy dust removal ash by using 20% dilute sulfuric acid, and removing slag to obtain a sulfate solution, wherein the sulfate comprises manganese sulfate, calcium sulfate, aluminum sulfate and magnesium sulfate;

step two: adjusting the concentrations of calcium sulfate, aluminum sulfate and magnesium sulfate in the sulfate solution to enable the calcium sulfate, the aluminum sulfate and the magnesium sulfate to generate calcium-magnesium-alum coprecipitation, then adding a certain amount of manganese powder, and separating the calcium-magnesium-alum to obtain a manganese sulfate solution;

step three: crystallizing the manganese sulfate solution obtained in the second step at a high temperature, and separating a crystal to obtain manganese sulfate;

step four: drying the manganese sulfate obtained in the third step, and then burning the manganese sulfate and sulfur together in an oxygen atmosphere to obtain manganese monoxide and sulfur dioxide;

step five: reacting sulfur dioxide with oxygen to generate sulfur trioxide by taking vanadium pentoxide as a catalyst;

step six: the sulfur trioxide reacts with water to produce sulfuric acid.

The method of the invention utilizes waste dilute sulfuric acid to treat the silicon-manganese alloy dedusting ash, can effectively recover manganese element in the silicon-manganese alloy dedusting ash to prepare manganese monoxide and sulfuric acid as by-product, can also effectively utilize the waste dilute sulfuric acid, can use calcium-magnesium alum as a raw material of a cement plant, realizes effective recovery and reutilization of resources, purifies a manganese sulfate solution through two reactions of coprecipitation and replacement to obtain high-purity manganese sulfate, utilizes the manganese sulfate and sulfur to be combusted together in an oxygen atmosphere, can directly generate the manganese monoxide, does not need to additionally consume heat energy, and saves energy resources.

Drawings

Fig. 1 is a schematic structural view of the silicon carbide lining baking furnace.

Fig. 2 is a partial view of the silicon carbide liner firing furnace.

FIG. 3 is a schematic structural diagram of the continuous high-temperature high-pressure crystallizer.

FIG. 4 is a sectional view of the continuous high-temperature high-pressure crystallizer taken along the direction A-A.

FIG. 5 is a sectional view of the continuous high-temperature high-pressure crystallizer taken along the direction B-B.

In the figure: the continuous high-temperature and high-pressure crystallizer comprises a silicon carbide lining roasting furnace 10, a furnace body 11, a shell 111, an aeration hole 1111, an aeration pipe 1112, an anticorrosive layer 112, a partition plate 113, a hood 114, a wind shield 115, a blower 12, a blast pipe 121, a cyclone separator 13, a circulating fan 14, a continuous high-temperature and high-pressure crystallizer 30, a pipe body 31, a crystallization liquid inlet 311, a first mother liquid port 312, a second mother liquid port 313, a third mother liquid port 314, a crystallization product outlet 315, a safety outlet 316, a safety valve 317, a third valve 318, a fourth valve 319, a heat exchanger 32, a heating component 33, a heat transfer oil inlet 331, a heat transfer oil outlet 332, a first valve 333, a second valve 334, a storage tank 34, a booster pump 35, a fifth valve 351 and a sixth valve 352.

Detailed Description

In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to these drawings without creative efforts.

The embodiment of the invention provides a process for preparing battery-grade manganese oxide and by-product sulfuric acid by roasting high-purity manganese sulfate and sulfur, which comprises the following steps:

the method comprises the following steps: washing the low-grade silicon-manganese alloy dust removal ash by using 20% dilute sulfuric acid, and removing slag to obtain a sulfate solution, wherein the sulfate comprises manganese sulfate, calcium sulfate, aluminum sulfate and magnesium sulfate;

step two: adjusting the concentrations of calcium sulfate, aluminum sulfate and magnesium sulfate in the sulfate solution to enable the calcium sulfate, the aluminum sulfate and the magnesium sulfate to generate calcium-magnesium-alum coprecipitation, then adding a certain amount of manganese powder, and separating the calcium-magnesium-alum to obtain a manganese sulfate solution;

step three: crystallizing the manganese sulfate solution obtained in the second step at a high temperature, and separating a crystal to obtain manganese sulfate;

step four: drying the manganese sulfate obtained in the third step, and then burning the manganese sulfate and sulfur together in an oxygen atmosphere to obtain manganese monoxide and sulfur dioxide;

step five: reacting sulfur dioxide with oxygen to generate sulfur trioxide by taking vanadium pentoxide as a catalyst;

step six: the sulfur trioxide reacts with water to produce sulfuric acid.

The method can be used for preparing 20% dilute sulfuric acid by mixing waste dilute sulfuric acid and concentrated sulfuric acid, calcium sulfate, aluminum sulfate and magnesium sulfate solution can be added into sulfate solution to generate calcium-magnesium alum coprecipitation, on one hand, calcium, aluminum, magnesium and the like in the sulfate solution are removed through coprecipitation, on the other hand, manganese powder is added to perform replacement reaction, so that metal elements with metal activity surface before manganese in the sulfate solution are formed and deposited to be removed, and the high-purity manganese sulfate solution is obtained.

The method of the invention utilizes waste dilute sulfuric acid to treat the silicon-manganese alloy dedusting ash, can effectively recover manganese element in the silicon-manganese alloy dedusting ash to prepare manganese monoxide and sulfuric acid as by-product, can also effectively utilize the waste dilute sulfuric acid, can use calcium-magnesium alum as a raw material of a cement plant, realizes effective recovery and reutilization of resources, purifies a manganese sulfate solution through two reactions of coprecipitation and replacement to obtain high-purity manganese sulfate, utilizes the manganese sulfate and sulfur to be combusted together in an oxygen atmosphere, can directly generate the manganese monoxide, does not need to additionally consume heat energy, and saves energy resources.

Referring to fig. 1 to 2, further, in the fourth step, after the manganese sulfate obtained in the third step is dried, roasting together with sulfur in a silicon carbide lining roasting furnace 10, wherein the silicon carbide lining roasting furnace 10 comprises a furnace body 11 and a blower 12, the furnace body 11 is a sealed cylinder, the furnace body 11 comprises a shell 111, the inner wall of the shell 111 is coated with a rigid anticorrosive layer 112, the anticorrosive layer 112 is made of silicon carbide materials, a horizontal partition plate 113 is arranged in the barrel, the partition plate 113 divides the furnace body 11 into a reaction chamber and an air equalizing chamber from top to bottom, the air blower 12 comprises a blast pipe 121, one end of the blast pipe 121 is communicated with an inner cavity of the air equalizing chamber, the other end of the blast pipe 121 is connected with an outlet of the air blower 12, a plurality of air hoods 114 are arranged on the partition plate 113, the air hoods 114 are uniformly distributed on the partition plate 113, an air inlet of each air hood 114 is communicated with the air equalizing chamber, and an air outlet of each air hood 114 is.

In this embodiment, the highly-compressed air who comes from air-blower 12 gets into the air-equalizing chamber earlier, the air-equalizing chamber is as buffer space, can provide the high-pressure air of pressure stability for each hood 114, guarantee that the reaction material in furnace body 11 is in a stable fluidization state, avoid influencing the reaction process because pressure is unstable or inconsistent causes local overfluidization and local undercluidization, conical air-equalizing chamber, the high-pressure air gets into the back, the highly-compressed air of whirl can separate steam by a small amount, reduce some steam and get into furnace body 11, the fixed microparticle that carries in the highly-compressed air can also subside to the highly-compressed air of whirl, avoid blockking up hood 114.

In the embodiment, the silicon carbide anticorrosive coating 112 is used as the lining of the furnace body 11, so that the contact between dilute sulfuric acid condensed from furnace gas in the furnace body 11 when encountering water and the shell 111 can be effectively prevented, the furnace body 11 is corroded, and the high-temperature equipment suitable for preparing manganese monoxide by roasting manganese sulfate and sulfur at high temperature by using a solid fluidization technology is provided.

Referring to fig. 3 to 5, further, in the third step, the manganese sulfate solution is crystallized at high temperature in the continuous high-temperature high-pressure crystallizer 30, the continuous high-temperature high-pressure crystallizer 30 includes a tube 31, a heat exchanger 32, a heating element 33, and a storage tank 34, the tube 31 is a slender sealed cylinder, the tube 31 is vertically disposed, the heat exchanger 32 is disposed in the tube 31 and is close to the top wall of the tube 31, the heat exchanger 32 divides the inner cavity of the tube 31 into a buffer chamber and a crystallization chamber, the buffer section is located above the heat exchanger 32, the crystallization section is located below the heat exchanger 32, the inlet of the tube side of the heat exchanger 32 is communicated with the buffer chamber, the outlet of the tube side of the heat exchanger 32 is communicated with the crystallization chamber, the heating element 33 is installed at the lower part of the sidewall of the tube 31 to heat the inner cavity of the crystallization chamber, the inlet 311 of the crystallization liquid is provided at the upper part of, a first mother liquor port 312 is arranged at the lower part of the side wall of the pipe body 31, a second mother liquor port 313 and a third mother liquor port 314 are arranged on the side wall of the pipe body 31 between the first mother liquor port 312 and the crystallization liquor inlet 311, the first mother liquor port 312 is connected with the second mother liquor port 313 through a pipeline, the second mother liquor port 313 is connected with the inlet of the shell side of the heat exchanger 32, the outlet of the shell side of the heat exchanger 32 is connected with the third mother liquor port 314, and a crystallization product outlet 315 is arranged on the bottom wall of the pipe body 31.

In the embodiment, the mass percentage concentration of manganese sulfate before crystallization is about 30%, the heat exchanger 32 cools the mother liquor entering the shell pass, the temperature of the mother liquor can be ensured to be lower than 100 ℃, the heat exchanger 32 can be prevented from being blocked by crystal substances separated out in the shell pass, and heat energy can be effectively recovered.

In this embodiment, after continuously entering the buffer chamber of the tube 31, the manganese sulfate solution in the storage tank 34 is preheated by the heat exchanger 32, and at the same time, the mother liquor in the heat exchanger 32 can be cooled, and then the manganese sulfate solution passes through the tube pass of the heat exchanger 32 and enters the crystallization chamber of the tube 31, the crystallization chamber is heated to a high temperature by the heating part 33, manganese sulfate is crystallized, manganese sulfate crystals flow out from the crystal outlet 315 of the tube 31, and the crystallization mother liquor is cooled to a temperature below 100 ℃ through the shell pass of the heat exchanger 32 and then is discharged from the third mother liquor outlet 314, so that the continuous crystallization of the manganese sulfate solution is realized. The tube body 31 adopts a slender vertical structure, so that the liquid in the tube body 31 flows from bottom to near the laminar flow, the condition of back mixing of the liquid is avoided, and the crystallization efficiency is favorably improved.

Referring to fig. 3 to 5, the continuous high-temperature high-pressure crystallizer 30 further includes a pressure pump 35, an inlet of the pressure pump 35 is connected to an outlet of the storage tank 34, and an outlet of the pressure pump 35 is connected to the crystallization liquid inlet 311.

In this embodiment, the manganese sulfate solution in the tube 31 can be in a high pressure state by the pressure pump 35, which is beneficial to improving the crystallization efficiency.

Referring to fig. 3 to 5, a safety outlet 316 is further disposed on the top wall of the tube 31, and a safety valve 317 is installed on the safety outlet 316.

Referring to fig. 3 to 5, further, the heating member 33 is a heat conducting oil heating jacket disposed on the outer wall of the tube 31 and integrated with the tube 31, a sealed heating cavity is formed between the inner wall of the heat conducting oil heating jacket and the outer wall of the tube 31, and heat conducting oil flows through the heating cavity.

Referring to FIGS. 3 to 5, further, the pressure in the tube 31 is 18kg/cm2The temperature of the crystalline segment of the tube 31 is 200 ℃.

Further, in the step one, a certain amount of iron sulfide is added in the process of washing the low-grade silicon-manganese alloy dust removal ash by using 20% dilute sulfuric acid.

In the embodiment, the ferric sulfide is added into the sulfate solution, so that high-valence manganese in dust can be reduced into bivalent manganese, and the yield of manganese in the dust is greatly improved.

Further, 20% dilute sulfuric acid was prepared from sulfuric acid of different concentrations.

Further, the mother liquor obtained by separating the crystal in the third step is returned to the first step to prepare 20% dilute sulfuric acid.

In the embodiment, the mother liquor obtained by separating the crystal is returned to prepare 20% dilute sulfuric acid, so that the waste dilute sulfuric acid realizes closed-loop zero emission.

Further, the low-grade silicon-manganese alloy dust-removing ash contains 13-17% of metal manganese.

Referring to fig. 3 to 5, in an embodiment, the third mother liquor port 314 is higher than the second mother liquor port 313, and the mother liquor in the shell side of the heat exchanger 32 is in a low-in and high-out mode, which is beneficial to improving the heat exchange efficiency. A heat conducting oil inlet 331 and a heat conducting oil outlet 332 communicated with the heating chamber are formed in the outer wall of the heat conducting oil heating jacket, the heat conducting oil outlet 332 is formed higher than the heat conducting oil inlet 331, the heat conducting oil in the heat conducting oil heating jacket is in a low-in and high-out mode, which is beneficial to improving heat exchange efficiency, a first valve 333 and a second valve 334 are respectively installed on the heat conducting oil inlet 331 and the heat conducting oil outlet 332, a third valve 318 is installed on the third mother liquor port 314, a fourth valve 319 is installed on the crystal outlet 315, a fifth valve 351 is installed on a pipeline between the pressure pump 35 and the storage tank 34, and a sixth valve 352 is installed on a pipeline between the pressure pump 35 and the pipe body 31.

In a particular embodiment, the axis of the conduit between the first mother liquor port 312 and the second mother liquor port 313 is perpendicular to the horizontal.

In a specific embodiment, the pipeline between the first mother liquor port 312 and the second mother liquor port 313 is a double-layer pipeline, and heat conducting oil flows in an interlayer of the double-layer pipeline opposite to the mother liquor.

In one embodiment, the inner bottom wall of the tube 31 is tapered.

Referring to fig. 1 and 2, further, a first jacket integrated with the reaction chamber is provided on an outer wall of the reaction chamber, and a first heating element is installed in a cavity between the first jacket and the outer wall of the reaction chamber.

Referring to fig. 1 and 2, a second jacket integrated with the gas equalizing chamber is further arranged on the outer wall of the gas equalizing chamber, and a second heating element is arranged in a cavity between the second jacket and the outer wall of the gas equalizing chamber.

In this embodiment, the high-pressure air entering the furnace body 11 can be preheated when the gas-equalizing chamber is in a high-temperature state, so that the reaction efficiency is improved.

Referring to fig. 1 and 2, further, the reaction chamber includes an expansion section at an upper portion and a reaction section at a lower portion, and an inner diameter of the reaction section is smaller than that of the expansion section.

In the embodiment, the diameter of the expansion section of the reaction chamber is larger than that of the reaction section, furnace gas enters the expansion section from the reaction section, the speed of the furnace gas is reduced, and a small amount of manganese monoxide particles or unreacted manganese sulfate and sulfur mixed in the furnace gas return to the reaction section again to continue to react.

Referring to fig. 1 and 2, further, the junction between the reaction section and the expansion section is a bevel transition.

Referring to fig. 1 and 2, further, the top of the expanding section is one of a flat top, an arched top, and a conical top.

Referring to fig. 1 and 2, further, the middle part of the reaction chamber is a concave saddle-shaped cylinder.

Referring to fig. 1 and 2, further, a sulfur dioxide gas outlet is provided at the top of the reaction chamber, a solid phase return port is provided at the side of the reaction chamber, the silicon carbide lining baking furnace 10 further includes a cyclone separator 13, a gas phase inlet at the side of the cyclone separator 13 is connected to the sulfur dioxide gas outlet of the reaction chamber, and a solid phase outlet at the bottom of the cyclone separator 13 is connected to the solid phase return port of the reaction chamber.

In the embodiment, the particles such as manganese monoxide, manganese sulfate, sulfur and the like carried by the furnace gas enter the cyclone separator 13, the unreacted particles can continue to react in the high-temperature furnace gas in the cyclone separator 13, and then the particles such as manganese monoxide, manganese sulfate, sulfur and the like are separated and then returned to the furnace body 11, so that the reaction rate and the yield can be improved.

Referring to fig. 1 and 2, further, a circulating gas outlet is provided on the side wall of the expanded section of the reaction chamber, the silicon carbide lining baking furnace 10 further includes a circulating fan 14, an inlet of the circulating fan 14 is connected with the circulating gas outlet through a pipeline, and an outlet of the circulating fan 14 is communicated with the inner cavity of the gas equalizing chamber through a pipeline.

In the embodiment, part of high-temperature sulfur dioxide generated gas can be extracted to enter the gas homogenizing chamber and then enter the reaction chamber, so that the reaction efficiency is favorably improved.

Referring to fig. 1 and 2, further, a wind shield 115 is arranged in the expansion section of the reaction chamber, the wind shield 115 is vertically arranged, and the wind shield 115 is arranged opposite to the circulating gas outlet.

In this embodiment, in the process of returning a part of the furnace gas carrying particles such as manganese monoxide, manganese sulfate, sulfur and the like to the gas equalizing chamber, the gas meets the wind shield 115, the gas changes direction and bypasses the wind shield 115, and the particles such as manganese monoxide, manganese sulfate, sulfur and the like collide with the wind shield 115 under the action of inertia to settle, and then return to the furnace body 11 again.

In a specific embodiment, the solid phase outlet at the bottom of the cyclone 13 is connected to the solid phase return port of the reaction chamber by an inclined flow pipe or by an L-shaped pipe, and the horizontal section of the L-shaped pipe may have a certain amount of material accumulation, so that the sulfur dioxide gas in the cyclone 13 can be prevented from flowing back to the furnace body 11 from the L-shaped pipe.

In a specific embodiment, the solid phase return port of the reaction chamber is arranged at the position of the reaction chamber where the diameter of the saddle-shaped cylinder is the smallest, when the airflow in the reaction chamber flows upwards, the flow speed is the fastest at the solid phase return port, and the flow speed is reduced at the position above the solid phase return port, so that negative pressure is formed at the solid phase return port, and the accumulated material of the horizontal section of the L-shaped pipeline is pumped out into the furnace body 11.

In a specific embodiment, a plurality of inflation holes 1111 are formed on the housing 111, one end of the inflation hole 1111 is communicated with the cavity between the housing 111 and the anticorrosive coating 112, the other end of the inflation hole 1111 is communicated with one end of an inflation pipe 1112, and the other end of the inflation pipe 1112 is communicated with the blower pipe 121. High-pressure air in the blower 12 enters the cavity between the shell 111 and the anticorrosive layer 112 through the air charging hole 1111, so that the shell 111 of the furnace body 11 can be ensured to be at a relatively low temperature, the furnace body 11 is prevented from being damaged due to a high-temperature state for a long time, the heat insulation performance of the furnace body 11 can be improved, the cavity between the shell 111 and the anticorrosive layer 112 is in a micro-positive pressure environment, furnace gas is prevented from contacting the shell 111 or penetrating through the shell 111, and the problem of dilute sulfuric acid corrosion inside and outside the shell 111 can be effectively avoided.

In a specific embodiment, an axial horizontal air outlet is formed in the sidewall of the hood 114, a blocking piece is pressed on the outer end face of the air outlet, the blocking piece is vertically arranged, the lower end of the blocking piece is a free end, the upper end of the blocking piece is hinged to the hood 114, when the air in the hood 114 is sprayed out from the air outlet, the blocking piece is pushed open, when the air outlet is not sprayed out, the blocking piece falls down due to gravity, the air outlet is covered, and therefore the blockage of the hood 114 due to the fact that reaction powder in the furnace body 11 enters the hood 114 is prevented.

The steps in the method of the embodiment of the invention can be sequentially adjusted, combined and deleted according to actual needs.

The modules or units in the device of the embodiment of the invention can be combined, divided and deleted according to actual needs.

While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention.

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