CN113518502A - Method for rapidly preparing sulfur plasma based on plasma ionization - Google Patents

Method for rapidly preparing sulfur plasma based on plasma ionization Download PDF

Info

Publication number
CN113518502A
CN113518502A CN202110761178.8A CN202110761178A CN113518502A CN 113518502 A CN113518502 A CN 113518502A CN 202110761178 A CN202110761178 A CN 202110761178A CN 113518502 A CN113518502 A CN 113518502A
Authority
CN
China
Prior art keywords
sulfur
plasma
gas
temperature
powder
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202110761178.8A
Other languages
Chinese (zh)
Inventor
张国兴
庞仁杰
储学群
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shanghai Sanfu Engineering Technology Co ltd
Original Assignee
Shanghai Sanfu Engineering Technology Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shanghai Sanfu Engineering Technology Co ltd filed Critical Shanghai Sanfu Engineering Technology Co ltd
Priority to CN202110761178.8A priority Critical patent/CN113518502A/en
Publication of CN113518502A publication Critical patent/CN113518502A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05HPLASMA TECHNIQUE; PRODUCTION OF ACCELERATED ELECTRICALLY-CHARGED PARTICLES OR OF NEUTRONS; PRODUCTION OR ACCELERATION OF NEUTRAL MOLECULAR OR ATOMIC BEAMS
    • H05H1/00Generating plasma; Handling plasma
    • H05H1/24Generating plasma

Abstract

The invention relates to a method for rapidly preparing sulfur plasma based on plasma ionization, which comprises the following steps: argon is used as an arc starting medium, the argon is firstly introduced into a plasma generator, and after the arc is normally started, sulfur-containing gas is introduced into the plasma generator to prepare the sulfur plasma with the temperature of 500-. Compared with the prior art, the method has no problems of electrode consumption and pollution, does not need to be formed under the high vacuum condition, can quickly obtain the sulfur plasma with high concentration and large air quantity, meets the requirement of the industrial process on the reducing gas, and can be used as the industrial reducing gas (agent) for reducing and decomposing materials such as gypsum, waste sulfuric acid, manganese dioxide and the like. The invention has simple process and high generation speed, can realize large-scale device, and can continuously produce the high-purity gas reducing agent, namely the sulfur plasma airflow by utilizing solid or liquid sulfur.

Description

Method for rapidly preparing sulfur plasma based on plasma ionization
Technical Field
The invention belongs to the technical field of sulfur plasma preparation, and relates to a method for rapidly preparing sulfur plasma based on plasma ionization.
Background
Sulfur is an important basic chemical raw material, can be widely used for producing sulfur dioxide, sulfuric acid, carbon disulfide, insoluble sulfur and metal sulfides, and can also be used for reducing sulfate ores, sulfate industrial waste residues and industrial waste sulfuric acid to produce sulfur products with higher added values.
Physics of sulfurIs characterized in that the crystal is a light yellow orthorhombic crystal at normal temperature and is saddle-shaped S8Cyclic structure with melting point of 115.207-120 deg.C, ignition point of 250 deg.C, boiling point of 444.6 deg.C, and solid density of 1.96-2.07X 103kg/m3) Flash point 207 ℃. When the temperature changes, the three-state transformation of solid, liquid and gas can occur, namely orthorhombic crystals at the temperature of 30-95.39 ℃ and single mixed crystals at the temperature of 95.39-115.207 ℃; when heated to a temperature greater than 115 deg.C, the melting temperature is reached and the sulfur is converted from a solid state to an amorphous liquid, and at 159 deg.C, S8The ring structure of (a) begins to break into an open-chain structure forming a linear polysulfide macromolecule with a consequent increase in viscosity, usually 159 ℃ being also defined as the lowest polymerization temperature of the eight-membered ring; when the temperature reaches 160 ℃, the viscosity of the liquid is increased by about 100 times, the viscosity is maximum when the temperature reaches 190 ℃, the long chain starts to break when the liquid is continuously heated, the viscosity is reduced again, and the liquidity of the liquid sulfur at 130-152 ℃ reaches the optimal state; when the temperature reaches 444.6 ℃ and the gasification is started, sulfur has various atomic configurations in a gaseous state, and the following cracking equilibrium exists in the gaseous sulfur along with the temperature change:
Figure BDA0003149832360000011
volume percent at vaporization point at 444.6 ℃: s2 3.5%,S6 54.0%,S842.5 percent; 593.3 ℃ volume percent: s215.5%,S6 59.1%,S825.4 percent; volume percent at gasification point at 800 ℃: s2 97.0%,S6 2.9%,S80.1 percent; at a temperature of between 450 ℃ and 900 ℃, the sulfur gas is actually S2、S4、S6、S8With increasing temperature, there is a conversion of the polyatomic sulfur molecules to lower sulfur molecules, i.e. S, by energy absorption cracking8→S6→S4→S2→S1Sulfur vapor mainly composed of S at 800 ℃ or higher2The sulfur vapor is composed of S at 1400 deg.C or above2Cleavage to monoatomic S1And (4) converting. The activity of sulfur in different forms is greatly different, and the higher the temperature, the shorter the molecular chain and the higher the reaction activity.
The existing industrialized device adopts sulfur combustion to produce sulfur dioxideLiquid sulfur can be used as raw materials for most of sulfuric acid; when the sulfur is used for producing carbon disulfide, insoluble sulfur, metal sulfide, sulfate and waste sulfuric acid, the reaction speed, the reaction efficiency and the reaction yield of the gas sulfur are much higher than those of liquid or solid sulfur. In the existing technology for preparing high-temperature sulfur gas by heating and gasifying sulfur, high-purity high-temperature sulfur gas is quickly gasified by utilizing electric heating energy of liquid sulfur, qualified portland cement and sulphoaluminate cement products are prepared by decomposing cement raw materials containing gypsum by utilizing gas sulfur, the solid-solid prereduction reaction of the traditional carbon reduction (coke + calcium sulfate → CaS) is converted into the gas-solid reaction of the sulfur reduction method (sulfur gas + calcium sulfate → CaS) to realize that the prereduction reaction time is shortened to 5-45 seconds from 20-30 minutes, the temperature of the prereduction reaction is also reduced to 700-900 ℃ from 1000-1150 ℃, the effect and the advantage of reducing the gypsum by the thiocarbon are obvious, but the reaction of reducing the gypsum to the CaS by the sulfur gas is S at the prereduction reaction temperature of 700-900 DEG C4、S2Gas + calcium sulfate → CaS, the reaction is endothermic, and the temperature and heat balance of the reaction system can be maintained only by supplementing part of heat to the reaction system, if the reaction system can be changed into S1Gas or active S particles + calcium sulfate → CaS, the reaction is exothermic, the reaction time is shortened from 5 to 45 seconds to 0.001 to 5 seconds, and the reaction can be completed instantly. However, at temperatures of 1400 ℃ the sulphur gas is predominantly S1In the gaseous state, it is difficult to obtain such high temperatures with conventional heating methods, and there is no material for equipment piping that can withstand such high temperature sulfur corrosion.
Compared with sulfur gas, the sulfur plasma has huge active groups, and can reduce the activation energy of macroscopic reaction, accelerate the reaction speed and shorten the reaction time when in subsequent related reaction.
Chinese invention patent CN1176244C discloses a vacuum plasma sulfurizing method, which ionizes gaseous sulfur sublimated by heating into sulfur positive ions and forms sulfur plasma in about 800V DC electric field, but the method ionizes gaseous sulfur into sulfur positive ions and forms low-temperature vacuum sulfur plasma under the action of low-temperature, high-vacuum degree of 0.1-1Pa and 800-1000V DC electric field within 400 ℃ (35-120 ℃), the DC electric field will consume electrodes, the electrodes are replaced frequently, the cost is high, and the electrode material pollutes the plasma, the industrial application is metal surface plasma sulfurizing treatment, the sulfur ion quantity required by workpiece surface sulfurizing treatment is relatively less, the sulfur gasification temperature under normal pressure is 444.6 ℃, the realization of large amount of sulfur is difficult under low-temperature, high-vacuum degree of 35-120 ℃, the method is not suitable for sulfur plasma requiring high concentration, sulfur plasma, The consumption is large under normal pressure or micro negative pressure.
Chinese invention patent CN1048356C discloses an autogenous growth method of gallium arsenide surface microwave discharge passive film, which utilizes microwave glow discharge to generate sulfur plasma, but the method is still the surface treatment of the material, and the adopted microwave discharge is still in high vacuum 10-4Low concentration evaporation and plasmatization of sulfur powder at-10 Pa and low temperature of 60-150 deg.C, and sulfur vapor pressure in discharge region maintained at 10-210Pa, belonging to the working condition that a small amount of sulfur is evaporated and plasmized in high vacuum and low temperature, and forming a low-concentration and small-gas-amount working condition, and the working condition can be only used for processing the surface of a workpiece.
Disclosure of Invention
The invention aims to provide a method for rapidly preparing sulfur plasma based on plasma ionization. Under normal pressure or micro negative pressure, sulfur steam or sulfur-containing gas forms 500-2500 ℃ high-temperature sulfur plasma under the action of high-frequency electromagnetic induction or microwave of a plasma generator, the problems of electrode consumption and pollution do not exist, the high-vacuum sulfur plasma is not required to be formed, the high-concentration (50-100% sulfur volume concentration) and large-atmosphere sulfur plasma can be quickly obtained, the requirement of an industrial process on reducing gas is met, and the high-temperature sulfur plasma can be used as industrial reducing gas (agent) for reducing and decomposing materials such as gypsum, waste sulfuric acid, manganese dioxide and the like or used as raw materials for producing carbon disulfide and metal oxides. The invention has simple process and high generation speed, can realize large-scale device, and can continuously produce the high-purity gas reducing agent, namely the sulfur plasma airflow by utilizing solid or liquid sulfur.
The purpose of the invention can be realized by the following technical scheme:
a method for rapidly preparing sulfur plasma based on plasma ionization comprises the following steps: argon is used as an arc starting medium, the argon is firstly introduced into a plasma generator, and after the arc is normally started, sulfur-containing gas is introduced into the plasma generator to prepare the sulfur plasma with the temperature of 500-.
Preferably, the residence time of the sulphur-containing gas in the plasma generator is between 0.001 and 15 seconds.
Further, the plasma generator adopts one or more combination of microwave discharge mode or high-frequency induction-coupling discharge mode.
Further, the sulfur-containing gas is high-temperature sulfur gas or mixed gas containing sulfur powder; and inert gas is used as carrier gas flow in the mixed gas containing the sulfur powder.
Further, the preparation method of the high-temperature sulfur gas comprises the following steps: heating and melting solid or liquid sulfur into crude sulfur liquid, filtering to obtain refined sulfur liquid, and heating and gasifying to obtain high-temperature sulfur gas. The heating gasification is one or more of a medium-frequency induction heating mode, a microwave heating mode and a resistance heating mode.
Further, the heating and melting temperature is 120-160 ℃ for 1-30 minutes, and the heating and gasifying temperature is 440-900 ℃, preferably 500-700 ℃ for 0.1-20 seconds.
Further, the preparation method of the mixed gas containing the sulfur powder comprises the following steps: crushing the solid sulfur (under the protection of inert gas) into sulfur powder, and then mixing the sulfur powder with carrier gas flow by taking the inert gas as carrier gas flow to obtain mixed gas containing sulfur powder.
Further, the solid sulfur is mechanically crushed or frozen and crushed by liquid nitrogen, and the particle size of the sulfur powder is-100 meshes and is more than or equal to 90 percent.
Furthermore, the outer wall of the plasma generator is made of one or more of quartz glass, silicon carbide and ceramic materials.
Furthermore, the plasma generator adopts a circulating cooling water indirect cooling mode to carry out outer wall external protection, and adopts sulfur gas or inert gas as outer wall internal protection cooling gas.
Furthermore, the sulfur plasma contains active groups with catalytic reduction effect.
The invention aims to convert sulfur gas S in the prior art into sulfur gas S by plasma treatment of sulfur2-S8Converting into sulfur plasma flow active groups; compared with sulfur gas S2-S8Electrically active groups S, S, S in the sulfur plasma2The sulfur particles and sulfur gas S have strong adsorption, permeation and collision effects in the contact reaction process of the sulfur particles and the raw materials of carbon, metal, gypsum, waste sulfuric acid and the like in a suspension dispersion state2-S8Compared with the prior art, the method has the advantages that the chemical activity strength is much higher, the particle size is smaller, the activation energy of macroscopic reaction is obviously reduced, the reaction which is very slow and difficult to carry out under certain conventional conditions becomes very easy, the reaction equilibrium temperature is reduced, the reaction time is instantly completed within 0.001-5 seconds from 5-45 seconds, the size of a reactor can be reduced from 1/9-1/50, the reaction efficiency and the production efficiency can be improved, the heat balance of a reaction system is facilitated, and a new way is found for the efficient recycling of industrial by-product gypsum, waste sulfuric acid, semi-coke powder and other materials.
Compared with the prior art, the invention has the following characteristics:
1. the process technology is complete, the heating ionization is rapid and stable, the arc is started by adopting argon firstly, and the operation is switched to the operation of working medium sulfur gas when the flame of the argon ionization arc is normal, so that the problem of difficult arc starting of the sulfur-containing gas is effectively solved.
2. The sulfur plasma is generated by adopting microwave discharge and high-frequency induction-coupling discharge modes, so that the electrode consumption is avoided, the problem of corrosion of sulfur to the electrode at high temperature is solved, the sulfur plasma atmosphere is pure, and the service life of the plasma generator is long.
3. The adjustment of the power load of the plasma power supply from 0-100% can be completed instantly, the change requirement of the increase of the instant heat load during sulfur plasmatization can be met, the change adjustment of the production load is convenient and flexible, the guarantee is provided for maintaining the temperature in the plasma arc flame, and the rapid plasmatization of sulfur is realized.
4. The plasma generator adopts an independent power supply control device, the power of the power supply is adjusted and controlled by detecting the temperature of the plasma, and when the load of the sulfur plasma needs to be adjusted, the addition of the sulfur entering the system is adjusted and is automatically controlled in linkage with the temperature of the plasma and the power supply.
5. The outer wall of the plasma body is made of quartz glass, silicon carbide and ceramic materials, so that the plasma body has good sulfur corrosion resistance and good magnetic permeability. The circulating cooling water is used as an external protection cooling measure of the outer wall, and the gas sulfur or nitrogen or inert air without oxygen is used as an internal cooling protection measure of the outer wall, so that the outer wall material can be well protected, and the service life of the plasma generator can be effectively prolonged.
6. The sulfur is broken by adopting nitrogen protection, and nitrogen or oxygen-free air is adopted for conveying as a conveying carrier, so that the safety of a production system is ensured.
7. The plasma generator is a closed space, oxygen-containing air can be prevented from being mixed, and the reducing atmosphere of the active sulfur plasma can be effectively maintained.
8. The sulfur plasma is excited to contain active groups with reduction catalysis effect on related reactions, including free radicals, ionic states, excited states and the like, and is rich in S, S and S2Active particles such as C, N, e, a small amount of C, CH, H, OH and the like have stronger chemical activity than sulfur gas, the macroscopic activation energy of the reaction with carbon, sulfate, metal and oxide is obviously reduced, the reaction speed is high, the reaction time is short, and the production efficiency is high.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a process flow diagram of example 1;
FIG. 3 is a process flow diagram of example 2;
FIG. 4 is a process flow diagram of example 3;
FIG. 5 is a process flow diagram of example 4.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments. The present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the scope of the present invention is not limited to the following embodiments.
As shown in figure 1, the method for preparing the sulfur plasma based on the plasma ionization comprises the steps of utilizing argon as an arc starting medium, firstly introducing the argon into a plasma generator, and introducing sulfur-containing gas into the plasma generator after normal arc starting to prepare a sulfur plasma product. The temperature of the sulfur plasma is 500-2500 ℃, preferably 800-1500 ℃.
Wherein the sulfur-containing gas is high-temperature sulfur gas or mixed gas of sulfur-containing powder using nitrogen and inert gas without oxygen as carrier. The preparation process comprises the following steps:
the preparation method of the high-temperature sulfur gas comprises the following steps: heating solid or liquid sulfur to a temperature higher than 120 ℃ by adopting steam, heat conduction oil or electricity to melt the sulfur into crude sulfur liquid, conveying the crude sulfur liquid into a sulfur filter by a crude sulfur conveying pump to be filtered, conveying the outlet clear liquid which is refined sulfur liquid into a refined sulfur tank by a refined sulfur conveying pump, conveying the refined sulfur liquid into a closed gasifier by a refined sulfur conveying pump, atomizing by a spray head, and heating up to a temperature higher than 450 ℃ by electricity to gasify into sulfur gas. The electric heating is one or more of resistance heating, electric induction heating and microwave heating, and electric induction heating is preferably adopted. The optimum temperature of the sulfur liquid is 130-158 ℃ in the processes of conveying, filtering and spray head atomization. The temperature of the liquid sulfur is 440-900 ℃ by electrical heating gasification, and preferably 500-700 ℃.
The preparation method of the mixed gas containing the sulfur powder comprises the following steps: crushing solid sulfur into sulfur powder, performing gas-solid separation, putting the sulfur powder into a sulfur powder storage bin, and mixing the sulfur powder into mixed gas containing sulfur powder by using nitrogen or inert air without oxygen as carrier gas flow. The solid sulfur is crushed by one of mechanical crushing and liquid nitrogen freezing crushing. The granularity of the sulfur powder is-100 meshes and is more than or equal to 90 percent. And nitrogen is adopted for protection in the processes of crushing and separating the solid sulfur, so that the system safety is improved.
The plasma generator is one or more of microwave discharge and high-frequency induction-coupling discharge. The outer wall of the plasma generator adopts one or more of quartz glass or ceramic materials. The outer wall of the plasma generator adopts circulating cooling water to indirectly cool the outer protection, and adopts one of sulfur gas, nitrogen or inert air without oxygen as the cooling gas for the inner protection of the outer wall.
Further, the sulfur plasma is excited to contain active groups having a reduction catalytic effect on the relevant reaction. The active groups include free radicals, ionic states, excited states, etc., such as a plurality of S, S, S2Active particles such as, N, e, small amount of C, CH, H, OH, etc.
Example 1:
as shown in fig. 2, in the technical scheme of this embodiment, solid sulfur is used as a raw material, the raw material is indirectly heated and melted by a steam coil to form liquid sulfur, a crude sulfur pump is used for pumping sulfur filter to remove solid and organic impurities, the filtered refined liquid sulfur is stored in a refined sulfur storage tank, the sulfur amount is controlled by a refined sulfur pump and a flowmeter, the sulfur is sent to a sulfur inlet atomizing nozzle of a gasification furnace, a high-temperature sulfur gas is obtained by heating and gasifying the sulfur gas by the gasification furnace, and the high-temperature sulfur gas is sent to a plasma generator under the normal argon arc starting condition to prepare sulfur plasma.
The liquid sulfur gasification selects medium frequency induction heating, the gas sulfur plasma selects high frequency induction-coupled discharge plasma generator, the outer wall material of the plasma generator adopts quartz glass, in order to protect the outer wall of the quartz glass of the plasma generator from being damaged by heat of high temperature arc flame, inert gas without oxygen is adopted as cooling protective gas inside the outer wall of the quartz glass, a cooling water channel is arranged outside the quartz glass wall, and circulating cooling is adopted together with the medium frequency coil, the high frequency coil, the medium and high frequency power supply and the like, so that the long-period stable operation of the medium frequency gasification furnace and the high frequency induction water cooling plasma generator in a safe temperature range is ensured.
The concrete application is as follows: adding solid sulfur into sulfur melting tank at 15 t/hr, heating to over 1 deg.c under the action of steam coilAt 18 deg.C, the solid is melted into liquid, and with the temperature further increased to 152 deg.C, the fluidity of the liquid sulfur reaches the optimum state, and the liquid sulfur is fed into sulfur filter via crude sulfur pump for filtration to remove solid impurities in sulfur, and the obtained refined liquid sulfur is fed into refined sulfur tank for buffer storage, and steam heating is performed to maintain the temperature of the refined sulfur tank at 140-3And h, and delivering the sulfur to a sulfur atomizing nozzle arranged at the feed end of the gasification furnace.
The gasification furnace adopts intermediate frequency power supply electric induction heating, and the power supply power is adjusted to control the internal temperature at 500-700 ℃. Under the temperature environment, the liquid sulfur fog drops sprayed by sulfur atomization are heated and rapidly heated to the temperature of 440-3The sulfur plasma product is sprayed into a subsequent relevant reaction system for use. The mole fraction of sulfur in the plasma generator outlet gas product is 70-90%.
The system operation and temperature control are realized by PLC, and the flow of the liquid sulfur, the internal temperature of the gasification furnace, the internal temperature of the plasma generator and the power of the control power supply are automatically controlled.
Example 2:
as shown in fig. 3, in the technical scheme of this embodiment, liquid sulfur is used as a raw material, heat preservation is performed by indirect heating through heat conduction oil or electricity to maintain molten liquid sulfur, solid and organic impurities are removed by filtering a crude sulfur pump with a sulfur filter, refined liquid sulfur after filtering is stored in a refined sulfur storage tank, the amount of sulfur is controlled by adjusting a refined sulfur pump and a flow meter, and is sent to a sulfur inlet atomizing nozzle of a gasification furnace, high-temperature sulfur gas is obtained by heating and gasifying through the gasification furnace, and then the high-temperature sulfur gas is sent to a plasma generator under the normal condition of argon arc starting to prepare sulfur plasma.
The liquid sulfur gasification selects high-frequency microwave heating, the gas sulfur plasma selects a high-frequency microwave discharge plasma generator, the outer wall material of the plasma generator adopts ceramic non-metallic material, in order to protect the ceramic outer wall of the plasma generator from being damaged by high-temperature arc flame heat, nitrogen is adopted as cooling protective gas in the ceramic outer wall, a high-frequency power supply, a microwave generating source and the like adopt circulating cooling water for cooling, and the long-period stable operation of the microwave gasification furnace and the high-frequency microwave plasma generator in a safe temperature range is ensured.
The concrete application is as follows: mixing liquid sulfur to 16m3Adding into a liquid sulfur storage tank, maintaining the temperature of the liquid sulfur at 135-3And h, and delivering the sulfur to a sulfur atomizing nozzle arranged at the feed end of the gasification furnace.
The gasification furnace is heated by high-frequency microwave, and the power of a power supply is adjusted to control the internal temperature to be 500-650 ℃. Under the temperature environment, liquid sulfur fog drops sprayed by sulfur atomization are heated to be rapidly heated to 440-3The sulfur plasma product is sprayed into a subsequent relevant reaction system for use. The mole fraction of sulfur in the plasma generator outlet gas product is 75-95%.
The system operation and temperature control are realized by DCS, and the liquid sulfur flow, the internal temperature of the gasification furnace, the internal temperature of the plasma generator and the power of the control power supply are automatically controlled.
Example 3:
as shown in fig. 4, in the technical scheme of this embodiment, solid sulfur is used as a raw material, sulfur powder with a particle size of-100 meshes or more than 90% is obtained by mechanical crushing and protection of oxygen-free inert air, the crushed sulfur powder is subjected to bag-type dust removal to obtain solid sulfur powder, the solid sulfur powder is stored in a powder bin, and the oxygen-free inert air discharged by a dust remover is recycled in a system; the sulfur powder in the powder bin is fed into a feeder and weighed, then the oxygen-free inert air is used as a carrier to form mixed gas containing sulfur powder, a plasma generator is started, and the sulfur-containing gas is fed into the powder bin under the normal condition of starting an arc by using argon to prepare sulfur plasma.
The high-frequency induction discharge plasma generator is selected for plasma gasification of sulfur-containing gas, the outer wall of the plasma generator is made of silicon carbide nonmetal materials, in order to protect the outer wall of silicon carbide of the plasma generator from being damaged by high-temperature arc flame heat, sulfur-containing gas or oxygen-free inert air is used as cooling protective gas inside the outer wall, a cooling water channel is arranged outside the outer wall, and the high-frequency induction plasma generator and a high-frequency coil and a power supply and the like are cooled by circulating cooling water, so that the long-period stable operation of the high-frequency induction plasma generator in a safe temperature range is ensured.
The concrete application is as follows: adding solid sulfur to a mechanical crusher for 6 tons/hour, obtaining sulfur powder with the granularity of-100 meshes which is more than or equal to 90 percent under the protection of nitrogen or inert air without oxygen, separating the sulfur powder by a bag-type dust collector to obtain solid sulfur powder, recycling the inert air without oxygen discharged by the dust collector in the system, and supplementing the inert air at regular time to ensure that the system does not contain oxygen; weighing the sulfur powder in the powder bin by a feeder to 5.5 tons/hour, forming mixed gas containing the sulfur powder by using nitrogen or inert air without oxygen as a carrier, starting a plasma generator, and feeding the sulfur-containing gas under the normal condition of starting arc by using argon to prepare 600-plus-material 2500 ℃ C and 4800-7700 Nm-plus-material3The sulfur plasma product is sprayed into a subsequent relevant reaction system for use. The mole fraction of sulfur in the plasma generator outlet gas product is 50-80%.
The system operation and temperature control are realized by DCS, and the solid sulfur amount, the internal temperature of the plasma generator and the power of the control power supply are automatically controlled.
Example 4:
as shown in fig. 5, in the technical scheme of the embodiment, solid sulfur is used as a raw material, sulfur powder with the particle size of-100 meshes which is larger than or equal to 90% is obtained by freezing and crushing with liquid nitrogen, the crushed sulfur powder is subjected to bag-type dust removal to obtain solid sulfur powder, the solid sulfur powder enters a powder bin for storage, and nitrogen discharged by a dust remover is recycled in a system; and (3) after the sulfur powder in the powder bin is fed by a feeder and weighed, nitrogen is used as a carrier to form mixed gas containing sulfur powder, a plasma generator is started, and the sulfur-containing gas is fed under the normal condition of argon arc starting to prepare sulfur plasma.
The high-frequency microwave discharge plasma generator is selected for plasma gasification of sulfur-containing gas, the outer wall of the plasma generator is made of ceramic nonmetal materials, in order to protect the ceramic outer wall of the plasma generator from being damaged by high-temperature arc flame heat, the sulfur-containing gas or nitrogen is used as cooling protective gas in the ceramic outer wall, and a high-frequency coil, a power supply and the like are cooled by circulating cooling water, so that the microwave plasma generator is ensured to operate stably for a long period in a safe temperature range.
The concrete application is as follows: adding solid sulfur to a freezing crusher for 4.5 tons/hour, obtaining sulfur powder with the granularity of-100 meshes and more than or equal to 90 percent under the protection of nitrogen, separating by a bag-type dust collector to obtain solid sulfur powder, recycling nitrogen discharged by the dust collector in a system, and supplementing nitrogen at regular time to ensure that no oxygen is contained in the system; the sulfur powder in the powder bin is weighed by a feeding machine for 4 tons/hour, nitrogen is used as a carrier to form mixed gas containing the sulfur powder, and the mixed gas is fed into the sulfur-containing gas under the normal condition of argon arc starting to prepare 600-1500 ℃ and 3500-5600 Nm-one3The sulfur plasma product is sprayed into a subsequent relevant reaction system for use. The mole fraction of sulfur in the plasma generator outlet gas product is 50-85%.
The system operation and temperature control are realized by PLC, and the solid sulfur amount, the internal temperature of the plasma generator and the power of the control power supply are automatically controlled.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.

Claims (10)

1. A method for rapidly preparing sulfur plasma based on plasma ionization is characterized by comprising the following steps: argon is used as an arc starting medium, the argon is firstly introduced into a plasma generator, and after the arc is normally started, sulfur-containing gas is introduced into the plasma generator to prepare the sulfur plasma with the temperature of 500-.
2. The method of claim 1, wherein the plasma generator employs one or both of a microwave discharge method and a high frequency induction-coupled discharge method.
3. The plasma ionization-based method for rapidly preparing sulfur plasma according to claim 1, wherein the sulfur-containing gas is high-temperature sulfur gas or a mixed gas containing sulfur powder; and inert gas is used as carrier gas flow in the mixed gas containing the sulfur powder.
4. The method for rapidly preparing sulfur plasma based on plasma ionization according to claim 3, wherein the preparation method of the high-temperature sulfur gas comprises the following steps: heating and melting solid or liquid sulfur into crude sulfur liquid, filtering to obtain refined sulfur liquid, and heating and gasifying to obtain high-temperature sulfur gas.
5. The method as claimed in claim 4, wherein the temperature for melting by heating is 160 ℃ and the temperature for vaporizing by heating is 900 ℃ respectively.
6. The method for rapidly preparing sulfur plasma based on plasma ionization according to claim 3, wherein the method for preparing the mixed gas containing sulfur powder comprises the following steps: crushing the solid sulfur into sulfur powder, then taking inert gas as carrier gas flow, and mixing the sulfur powder and the carrier gas flow to obtain mixed gas containing sulfur powder.
7. The method for rapidly preparing sulfur plasma based on plasma ionization according to claim 6, wherein the solid sulfur is crushed mechanically or frozen by liquid nitrogen, and the particle size of the sulfur powder is-100 meshes or more than 90%.
8. The method of claim 1, wherein the outer wall of the plasma generator is made of one or more of quartz glass, silicon carbide, and ceramic materials.
9. The method for rapidly preparing sulfur plasma based on plasma ionization as claimed in claim 1, wherein the plasma generator is protected outside the outer wall by indirect cooling with circulating cooling water, and sulfur gas or inert gas is used as the cooling gas for protecting inside the outer wall.
10. The method for rapidly preparing sulfur plasma based on plasma ionization according to claim 1, wherein the sulfur plasma contains active groups with catalytic reduction effect.
CN202110761178.8A 2021-07-06 2021-07-06 Method for rapidly preparing sulfur plasma based on plasma ionization Pending CN113518502A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110761178.8A CN113518502A (en) 2021-07-06 2021-07-06 Method for rapidly preparing sulfur plasma based on plasma ionization

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110761178.8A CN113518502A (en) 2021-07-06 2021-07-06 Method for rapidly preparing sulfur plasma based on plasma ionization

Publications (1)

Publication Number Publication Date
CN113518502A true CN113518502A (en) 2021-10-19

Family

ID=78066596

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110761178.8A Pending CN113518502A (en) 2021-07-06 2021-07-06 Method for rapidly preparing sulfur plasma based on plasma ionization

Country Status (1)

Country Link
CN (1) CN113518502A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115818580A (en) * 2022-11-28 2023-03-21 华中科技大学 Method for preparing nano sulfur material by using dielectric barrier discharge plasma and product

Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5211923A (en) * 1991-08-01 1993-05-18 University Of Chicago Hydrogen and sulfur recovery from hydrogen sulfide wastes
JP2001077093A (en) * 1999-09-06 2001-03-23 Shibaura Mechatronics Corp Dry etching method
CN2451602Y (en) * 2000-11-06 2001-10-03 北京金东方科技发展有限公司 Active sulphion generator using for sulphurizing process
US6398125B1 (en) * 2001-02-10 2002-06-04 Nanotek Instruments, Inc. Process and apparatus for the production of nanometer-sized powders
CN103657370A (en) * 2012-09-07 2014-03-26 韩国能量技术研究院 Device and method for removing hydrogen sulphide and carbonyl sulphide by virtue of microwave plasmas
CN103769594A (en) * 2013-11-25 2014-05-07 王利民 Technological method and device for preparing high-purity spherical superfine/nanoscale powdered materials in plasma atomization mode
KR101400669B1 (en) * 2012-12-27 2014-05-29 한국기초과학지원연구원 Gasification device of solid hydrocarbon using microwave plasma torch
WO2018034413A1 (en) * 2016-08-18 2018-02-22 주식회사 제이몬 Deposition device provided with plasma activation device
CN109019522A (en) * 2018-07-24 2018-12-18 上海三夫工程技术有限公司 The technique of high-purity sulfur gas is quickly produced based on electrical induction
CN109665507A (en) * 2018-10-12 2019-04-23 四川大学 Utilize the method and its implementing device of plasma-based Traffic Decomposition sulphur phosphorus system material

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5211923A (en) * 1991-08-01 1993-05-18 University Of Chicago Hydrogen and sulfur recovery from hydrogen sulfide wastes
JP2001077093A (en) * 1999-09-06 2001-03-23 Shibaura Mechatronics Corp Dry etching method
CN2451602Y (en) * 2000-11-06 2001-10-03 北京金东方科技发展有限公司 Active sulphion generator using for sulphurizing process
US6398125B1 (en) * 2001-02-10 2002-06-04 Nanotek Instruments, Inc. Process and apparatus for the production of nanometer-sized powders
CN103657370A (en) * 2012-09-07 2014-03-26 韩国能量技术研究院 Device and method for removing hydrogen sulphide and carbonyl sulphide by virtue of microwave plasmas
KR101400669B1 (en) * 2012-12-27 2014-05-29 한국기초과학지원연구원 Gasification device of solid hydrocarbon using microwave plasma torch
CN103769594A (en) * 2013-11-25 2014-05-07 王利民 Technological method and device for preparing high-purity spherical superfine/nanoscale powdered materials in plasma atomization mode
WO2018034413A1 (en) * 2016-08-18 2018-02-22 주식회사 제이몬 Deposition device provided with plasma activation device
CN109019522A (en) * 2018-07-24 2018-12-18 上海三夫工程技术有限公司 The technique of high-purity sulfur gas is quickly produced based on electrical induction
CN109665507A (en) * 2018-10-12 2019-04-23 四川大学 Utilize the method and its implementing device of plasma-based Traffic Decomposition sulphur phosphorus system material

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115818580A (en) * 2022-11-28 2023-03-21 华中科技大学 Method for preparing nano sulfur material by using dielectric barrier discharge plasma and product

Similar Documents

Publication Publication Date Title
KR101290659B1 (en) Preparation method of silicon oxide powder using thermal plasma, and the silicon oxide powder thereby
Li et al. Review of resource and recycling of silicon powder from diamond-wire sawing silicon waste
WO2015015795A1 (en) Siox powder manufacturing process and siox powder manufacturing apparatus
CN114031082B (en) Method for preparing nano silicon powder by induction plasma pyrolysis of silane
KR20150017795A (en) Apparatus for purification of graphite using a microwave plasma and the method for purification thereof
CN113518502A (en) Method for rapidly preparing sulfur plasma based on plasma ionization
TW201031590A (en) Plant for producing silicon with improved resource utilization
CN110540208A (en) Method for producing silicon
CN102001661B (en) Method for slagging, boron removal and purification of metalluragical silicon
CN103589459B (en) Coal gasification method and device employing plasma torch heating technology
CN101357750B (en) Method and device of microwave excitation molten salt catalytic reforming gasification carbon group compound
CN102275929A (en) Method for improving purity of metallurgical silicon and apparatus for realizing method
CN113336196A (en) Gasification cracking device based on microwave heating and method for rapidly preparing sulfur gas
CN103570023A (en) Slag-making and boron-removing method for industrial silicon
CN101181997A (en) Method for preparing metallic silicon material
Yang et al. A new strategy for de-oxidation of diamond-wire sawing silicon waste via the synergistic effect of magnesium thermal reduction and hydrochloric acid leaching
US8754001B2 (en) Self sustained system for sorbent production
CN218089652U (en) Plasma-assisted ammonia direct reduction smelting device
CN113148960B (en) Method for preparing high-purity sulfur-containing product from molybdenum concentrate in short process
US6207024B1 (en) Method of preparing phosphorus
CN201276417Y (en) Apparatus for catalytic reforming gasification of carbon based compound by microwave excitation molten salt
CN113477198B (en) Gasification cracking device based on electric induction heating and method for preparing sulfur gas
WO2009065444A1 (en) A method of producing polycrystalline and single crystal silicon
KR102508756B1 (en) Device for producing acetylene black using complexing a plasma treatment and a thermal decomposition
Nomura Fuel Production and Materials Synthesis by In-liquid Plasma

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination