Apparatus and method for producing treatment agent containing polysulfide

Abstract

To accurately, safely and continuously produce a treatment agent containing a polysulfide produced by reacting sulfur, an alkali compound and water.SOLUTION: An apparatus for producing a treatment agent containing a polysulfide has a mixing device for mixing a raw material composed of sulfur, an alkali compound and water at a predetermined mixing ratio, a supply device for storing a raw material mixed by the mixing device, and supplying the raw material by a predetermined amount, a reaction device for reacting the raw material supplied from the supply device at a predetermined pressure and a predetermined temperature, and producing a treatment agent containing a polysulfide, a cooling device for forcibly cooling a treatment agent produced by the reaction device, to a predetermined temperature, and a cushioning device for naturally radiating the treatment agent cooled by the cooling device to a predetermined temperature, and storing the treatment agent; and intermittently force-feeds the raw material and the treatment agent between each component, and continuously produces a treatment agent containing a polysulfide.SELECTED DRAWING: Figure 1

Description

[Technical field]

[0001] The present invention relates to an apparatus and method for producing a treatment agent containing a polysulfide. [Background technology]

[0002] Conventionally, treatment agents containing polysulfides as their main component have been widely used for various purposes such as insolubilizing heavy metals and fixing and decomposing asbestos.

[0003] The present inventors have developed a treatment agent containing polysulfides (particularly, Sx (x=6 to 12)) by reacting sulfur with an alkaline compound such as potassium hydroxide, magnesium hydroxide, calcium hydroxide, or sodium hydroxide, and water under high temperature and pressure (see, for example, Patent Document 1). [Prior art documents] [Patent documents]

[0004] [Patent Document 1] JP 2005-213375 A Summary of the Invention [Problem to be solved by the invention]

[0005] The present invention provides an apparatus and method for producing a treatment agent containing a polysulfide produced by reacting sulfur, an alkali compound, and water, accurately, safely, and continuously. [Means for solving the problem]

[0006] In the present invention according to claim 1, a manufacturing apparatus for a polysulfide-containing treatment agent includes a mixing device for mixing raw materials consisting of sulfur, an alkaline compound, and water in a predetermined mixing ratio, a supplying device for storing the raw materials mixed in the mixing device and supplying them in predetermined amounts, a reaction device for reacting the raw materials supplied from the supplying device at a predetermined pressure and a predetermined temperature to produce a polysulfide-containing treatment agent, a cooling device for forcibly cooling the treatment agent produced in the reaction device to a predetermined temperature, and a buffer device for allowing the treatment agent cooled in the cooling device to naturally dissipate heat to a predetermined temperature and store it, and the raw materials and treatment agent are intermittently pumped between the supplying device, the reaction device, and the cooling device to continuously produce the polysulfide-containing treatment agent.

[0007] In the present invention according to claim 2, the sulfur, the alkaline compound, and the water are mixed in the mixer while the sulfur and the alkaline compound are crushed in water.

[0008] In the present invention according to claim 3, the sulfur and the alkaline compound are crushed in water in the reaction device, while the sulfur, the alkaline compound, and water are reacted to produce the treating agent.

[0009] In the present invention according to claim 4, in the reaction device, the treatment agent is pressure-fed to the cooling device by using the increased pressure during the reaction.

[0010] In the present invention according to claim 5, in the cooling device, cooling is performed by mixing a previously produced cooled processing agent with a later produced uncooled processing agent.

[0011] In addition, in the present invention according to claim 6, in a method for producing a polysulfide-containing treatment agent, a treatment agent production device is used that includes a mixing device for mixing raw materials consisting of sulfur, an alkali compound, and water in a predetermined mixing ratio, a supplying device for storing the raw materials mixed in the mixing device and supplying them in predetermined amounts, a reaction device for reacting the raw materials supplied from the supplying device at a predetermined pressure and a predetermined temperature to produce a polysulfide-containing treatment agent, a cooling device for forcibly cooling the treatment agent produced in the reaction device to a predetermined temperature, and a buffer device for allowing the treatment agent cooled in the cooling device to naturally dissipate heat to a predetermined temperature and store it, and the raw materials and treatment agent are intermittently pumped between each device to continuously produce the polysulfide-containing treatment agent.

[0012] In addition, in the present invention according to claim 7, the manufacturing apparatus according to claim 6 uses sulfur and water, or sulfur, water and an alkaline compound, as raw materials, and processes them in a reaction apparatus at a temperature below the melting point of sulfur to produce a sulfur-containing material, and the produced sulfur-containing material is added to the treatment agent produced by the manufacturing method according to claim 6. Effect of the Invention

[0013] According to the present invention, a treatment agent containing polysulfides formed by reacting sulfur, an alkali compound, and water can be produced continuously, accurately, safely, and efficiently. [Brief description of the drawings]

[0014] [Figure 1] FIG. 2 is an explanatory diagram showing an apparatus for producing a treatment agent containing a polysulfide. [Diagram 2] FIG. 2 is an explanatory diagram showing a method for producing a treatment agent containing a polysulfide. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0015] Hereinafter, specific configurations of an apparatus and method for producing a treatment agent containing a polysulfide according to the present invention will be described with reference to the drawings.

[0016] As shown in FIG. 1, the production apparatus 1 is provided with a mixer 2, a feeder 3, a reactor 4, a cooler 5, and a buffer 6.

[0017] Each device (mixer 2, feeder 3, reactor 4, cooler 5, buffer 6) can be sealed and is connected by delivery pipes 7, 8, 9, 10. Control valves 11, 12, 13, 14 are provided in the delivery pipes 7, 8, 9, 10, respectively.

[0018] In addition, a compressor 15 is connected to the supply device 3 and the reaction device 4 via distribution pipes 16, 17, so that the high-pressure gas generated by the compressor 15 can be supplied to each device (supply device 3, reaction device 4) via each distribution pipe 16, 17. Each distribution pipe 16, 17 is provided with a control valve 18, 19.

[0019] Supply pipes 20, 21, and 22 for respectively supplying sulfur, an alkaline compound, and water, which are the raw materials for the treatment agent to be produced, are connected to the mixer 2. The supply pipes 20, 21, and 22 are provided with control valves 23, 24, and 25, respectively.

[0020] A supply pipe 26 for supplying the manufactured processing agent is connected to the buffer device 6. A control valve 27 is connected to the supply pipe 26.

[0021] A water source 28 for cooling each device (reactor 4, cooling device 5) from the outside is connected to the reaction device 4 and the cooling device 5 via a cooling water flow path 29, and a three-way valve 30 is provided at the upstream end of the cooling water flow path 29, while the downstream end of the cooling water flow path 29 is connected to a water supply pipe 22. The water supplied from the water source 28 is used as cooling water for cooling the cooling device 5 and the exhaust stack 31 of the reaction device 4, and is then supplied to the mixer 2 as raw water.

[0022] Each device (mixer 2, feeder 3, reactor 4, cooler 5, buffer 6, compressor 15) and each control valve 11, 12, 13, 14, 18, 19, 23, 24, 25, 27 and three-way valve 30 are controlled by a control device.

[0023] As shown in FIG. 2, this manufacturing apparatus 1 reacts predetermined amounts of raw materials, namely sulfur, an alkaline compound, and water, intermittently (for each batch) to continuously generate and provide a treatment agent (sulfur mixture).

[0024] First, in the mixer 2, raw materials consisting of sulfur, an alkaline compound, and water are mixed in a preset mixing ratio, and the mixed raw materials are allowed to flow down to the feeder 3 by gravity.

[0025] In this mixing device 2, sulfur and an alkaline compound are crushed underwater using a roller-type crusher or the like while mixing sulfur, an alkaline compound, and water, thereby reducing the diameter of the sulfur particles and improving their hydrophilicity and fluidity.

[0026] Here, the raw material sulfur is in the form of a lump or powder. The alkaline compounds used are potassium hydroxide, magnesium hydroxide, calcium hydroxide (slaked lime), sodium hydroxide, etc. The water used is recovered from a water source 28.

[0027] Next, the raw materials mixed in the mixer 2 are temporarily stored in the feeder 3, and are pumped (fed) to the reaction device 4 in predetermined amounts at a time.

[0028] The supply device 3 also functions as a receiver to prevent the high-pressure treatment agent from scattering when a problem occurs in the reaction device 4, etc.

[0029] Next, in the reaction device 4, the raw material supplied from the supply device 3 is reacted at a predetermined pressure and a predetermined temperature set in advance to produce a treatment agent containing polysulfides, and the produced treatment agent is pumped to the cooling device 5.

[0030] In this reaction device 4, a roller-type crusher or the like is used to crush sulfur and alkaline compounds underwater, while the sulfur, alkaline compounds, and water are reacted to produce a treatment agent, which separates the alkaline compounds attached to the sulfur particles from the sulfur and crushes the sulfur particles so that the reaction with the alkaline compounds can be carried out smoothly.

[0031] This reaction device 4 has a burner installed below a sealed pressure vessel and an exhaust pipe 31 installed above it, and a heat recovery jacket that heats the pressure vessel with heat from the burner and flows into the exhaust pipe 31 around the outer periphery of the pressure vessel, and the heat recovery jacket is covered with a vacuum layer and a heat-insulating layer. Inside the pressure vessel, a liner plate to prevent crushing and thermal shock is laid on the boulders, and the raw materials are crushed and reacted with rollers that roll on the liner plate. A heat recovery pipe that flows cooling water is installed around the outer periphery of the exhaust pipe 31.

[0032] The reaction device 4 is configured to pump the treatment agent to the cooling device 5 using the rising pressure during the reaction. The treatment agent may be pumped to the cooling device 5 using only the rising pressure during the reaction, or the treatment agent may be pumped to the cooling device 5 using the pressure from the compression device 15 in combination.

[0033] Next, in the cooling device 5 , the processing agent produced in the reaction device 4 is forcibly cooled to a predetermined temperature that has been set in advance, and the cooled processing agent is pumped to the buffer device 6 .

[0034] In this cooling device 5, a processing agent that has been generated earlier and cooled to about 45°C is mixed with a processing agent that has been generated later and is at about 150°C before being cooled, by high-speed spraying, thereby cooling the processing agent that has been generated later to about 45°C.

[0035] This cooling device 5 is provided with a cooling cylinder that flows cooling water around the outer periphery of a sealed heat-resistant container, and sprays the treatment agent generated later onto the bottom of the heat-resistant container, while pressure-feeding the treatment agent generated earlier from the middle of the heat-resistant container to a buffer device 6.

[0036] The cooling device 5 also functions as a receiver to prevent the high-pressure treatment agent from scattering when a problem occurs in the reaction device 4, etc.

[0037] Next, in the buffer device 6 , the processing agent cooled in the cooling device 5 is allowed to naturally dissipate heat until it reaches a preset temperature, where it is stored, and the cooled processing agent is supplied from the supply pipe 26 .

[0038] This buffer device 6 is provided with an agitating blade inside a sealed heat-dissipating container, and is designed to naturally dissipate heat while agitating the treatment agent, making it possible to supply the treatment agent at a safe temperature (about 40° C.).

[0039] In the above-mentioned manufacturing apparatus 1, sulfur, an alkaline compound, and water are used as raw materials, and the reaction is carried out in a reaction apparatus 4 at about 150° C. and 2.5 to 10 kgf / cm 2 By reacting with the above, a liquid treating agent containing a polysulfide can be produced.

[0040] In the above-mentioned manufacturing apparatus 1, sulfur and water, or sulfur, an alkaline compound, and water are used as raw materials, and when the raw materials are processed in the reaction apparatus 4 without heating and pressurizing so that the temperature does not exceed the melting point of sulfur so as not to change the physical properties of sulfur, a solid sulfur-containing material immersed in water can be produced. In addition, the sulfur-containing material is preferably about 35% of the total (sulfur and water, or sulfur, water, and an alkaline compound) in consideration of storage safety. Sulfur and an alkaline compound are used in a ratio of about 2:1. The temperature of the processing (water) is preferably 70 to 80°C, because the alkaline compound dissolves at 70°C or lower, and sulfur dissolves or evaporates at 80°C or higher.

[0041] The sulfur-containing material produced in this manner by the manufacturing apparatus 1 can be safely stored without causing any change in the physical properties of the sulfur, and the dehydrated material can be used as a raw material to produce a treatment agent containing polysulfides using the manufacturing apparatus 1 and manufacturing method described above. Moreover, after dehydration, the added material can be added to the treatment agent containing polysulfides produced by the manufacturing apparatus 1 and manufacturing method described above, and the added material can be used as the treatment agent.

[0042] In the manufacturing apparatus 1 (manufacturing method), the above series of steps are performed intermittently and continuously as one batch approximately every 15 minutes, thereby accurately, safely and continuously producing a treatment agent containing polysulfides generated by reacting sulfur, an alkaline compound and water.

[0043] The treatment agent provided from the buffer device 6 can be separated into gas and liquid using a filter or the like, and can be used as a liquid treatment agent, a solid treatment agent, or a recovered raw material.

[0044] In the above-mentioned manufacturing apparatus 1 (manufacturing method), for example, when a treatment agent is produced by mixing calcium hydroxide, sulfur, and water, Ca(OH)2 →Ca ++ +2OH -- Ca ++ +S→CaS The reaction occurs: This CaS is 2CaS+4OH -- →H2S+Ca(OH)2+S+Ca+O2 It becomes.

[0045] By carrying out this reaction in a sealed container, no steam is emitted, so the reaction proceeds accurately. H2S+Ca(OH)2+S+Ca→Ca(HS)2+Ca(OH)2 It becomes.

[0046] In addition, CaS is 2CaS+2H2O→Ca(HS)2+Ca(OH)2 And, for CaS, CaS+(x-1)S→CaSx Thus, CaSx (x=6) is generated stably.

[0047] This is not limited to the case where calcium hydroxide is used, but even when potassium hydroxide, magnesium hydroxide, sodium hydroxide, or a mixture of these is used, a treatment agent containing Sx (x=6) can be stably produced.

[0048] In particular, a treatment agent mainly composed of polysulfides (wherein Sx (x=6)) can be produced more stably by reacting potassium hydroxide, magnesium hydroxide, calcium hydroxide, sodium hydroxide or a mixture of these with sulfur while stirring and mixing so as to crush and peel off the potassium, magnesium, calcium or sodium attached to the surface of sulfur particles.

[0049] In the manufacturing apparatus 1, before the start of manufacturing the treatment agent or after the end of manufacturing, cleaning water heated to about 80°C is passed through each device (mixing device 2, supply device 3, reaction device 4, cooling device 5, buffer device 6), delivery pipes 7, 8, 9, 10, supply pipe 26, etc., to wash and heat them. This makes it possible to prevent the raw material powder (especially sulfur) from adhering and remaining, and also makes it unnecessary to separately heat (keep warm) the delivery pipes 7, 8, 9, 10, etc. The cleaning water is heated to about 80°C when collected, and is effectively used as raw material water.

[0050] In the manufacturing apparatus 1, cooling water at about 15°C is passed through the cooling tube of the cooling device 5 and the heat recovery tube of the reaction device 4 to cool the treatment agent from about 150°C to about 80°C, and cool the exhaust gas from the burner of the reaction device 4 from about 180°C to about 90°C. The cooling water heated to about 40°C by this cooling is also recovered and effectively used as raw water.

[0051] When manufacturing a treatment agent using sulfur and alkaline compounds as raw materials, if a polysulfide compound is manufactured at a temperature range of approximately 95°C to 110°C, depending only on the dissolution temperature of sulfur, the dissolution characteristics of the raw material sulfur and alkaline compounds are in conflict with each other, so alkaline crystals adhere to the surface of the sulfur particles, preventing the dissolution of sulfur and leaving undissolved sulfur particles.

[0052] Therefore, in the present invention, the raw material is crushed and reacted under high temperature and pressure, thereby making it possible to prevent undissolved sulfur particles from remaining.

[0053] When the raw materials are reacted under such high temperatures and pressures, the solubility of sulfur is affected by the outflow of steam generated by the reaction, making it difficult to stably produce a high-concentration treatment agent.

[0054] Therefore, in the present invention, the reaction is carried out inside a sealed pressure-resistant container (reaction device 4), which prevents the escape of vapor during the reaction and enables the stable production of a high-concentration treatment agent.

[0055] When a high-temperature treatment agent is produced in this way, it must be cooled to a safe operating temperature (about 40°C), but if the cooling rate is slow, unreacted materials in the raw material (mainly impurities contained in alkaline compounds) and 25μm to 50μm sulfur particles generated in the heat dissipation area at the liquid surface of the treatment agent will become nuclei to generate spherical sulfur of about 100μm to 500μm. On the other hand, slight improvement can be achieved by adding a surfactant to the treatment agent, but only a low-concentration treatment agent with a sulfur dissolution ratio of about 10% to 12% can be produced, and unreacted dissolved particles will precipitate as a precipitate.

[0056] Therefore, in the present invention, the high-temperature treatment agent generated in the reaction device 4 is forcibly cooled at high speed in the cooling device 5, thereby preventing sulfur from remaining and preventing sulfur from adhering to the inside of the device and piping, causing blockages.

[0057] Moreover, in the present invention, by forcibly cooling the raw materials and processing agents while pumping them, the tact time (the processing time required for one batch) during production can be shortened, and the initial (first batch) processing raises the temperature inside the pipes, preventing blockage of the pipes from the second time onwards. For safety, the pipes may be kept warm.

[0058] As a result, the present invention can stably produce a treatment agent with a final sulfur solubility density of approximately 1.35 g / cc.

[0059] In addition, when the reaction is carried out under high temperature and pressure, the pressure vessel (reactor 4) is repeatedly subjected to a heat cycle of about 130°C, from a raw material temperature of 20°C to a treatment agent temperature of 150°C. Therefore, when using stainless steel, which has a lower thermal conductivity than iron, it is necessary to prevent thermal degradation.

[0060] Therefore, in the present invention, the temperature of the raw materials is raised to about 80°C when they are supplied by obtaining the raw material reaction water from the heat recovery line, the crushing liner plate is made of 40 kg of carbon steel liner plate with a certain heat capacity to function as a heat storage material, the mounting part is configured like a clog seat to absorb the thermal deformation of the can body, volcanic rock-based pebbles are filled between the can body and the liner plate as a heat storage material, the crushing rollers are made of carbon steel, and the pebbles, liner plate and rollers weigh 65 kg and function as a heat storage material other than the can body and shaft.

[0061] This makes it possible to raise the temperature to around 80°C immediately after the raw materials are added, improving thermal efficiency and productivity while keeping the temperature change to an extremely small, reassuring value.

[0062] In addition, in the cooling device 5, the treatment agent generated later is sprayed into the treatment agent generated earlier, thereby forcibly cooling the treatment agent at high speed. A liner plate is provided at the treatment agent spray outlet to form a swirling flow of the sprayed treatment agent, allowing the treatment agent to be cooled uniformly at high speed.

[0063] This allows the treatment agent produced at around 150°C to be rapidly cooled to a temperature below the temperature at which sulfur particles begin to grow, producing a treatment agent that maintains good liquid properties.

[0064] In addition, by crushing and pumping sulfur without dissolving it at 80°C or less (below the melting temperature) using the above manufacturing apparatus 1 so as not to change the physical properties of the raw material sulfur, it becomes possible to further mix an alkaline compound as necessary and use it in a blend with a sulfur mixture as a treatment agent with added functions such as maintaining high alkalinity and improving sterilization properties. In addition, when an alkaline compound is used in combination with the treatment agent to prevent asbestos from scattering or to suppress the scattering of the treated object, it is also possible to process gypsum board, desulfurized lime, etc. and use them as an admixture.

[0065] The treating agent according to the present invention can be used as an asbestos fixing agent, an asbestos decomposing agent, a heavy metal insolubilizing agent, an agricultural chemical, a bath additive, an auxiliary for blocking the growth of seaweed or algae, a soil improving agent, a rust inhibitor, and the like.

[0066] As described above, the present invention can prevent sulfur crystals from adhering to the inside of pipes and causing blockages as the concentration of sulfur contained in the treatment agent increases.

[0067] Furthermore, in the present invention, evaporation of the reaction water is prevented, and unreacted and recrystallized sulfur is suppressed, so that the amount of sulfur contained in the treatment agent can be adjusted to the blending value of the raw material.

[0068] Furthermore, the present invention can reduce the sulfur content contained in the precipitate that is generated during production and removed by filtration.

[0069] Furthermore, in the present invention, the increase in the particle size of sulfur in the treatment agent can be prevented, making it possible to keep the particle size at 30 μm or less.

[0070] Furthermore, in the present invention, the raw materials and processing agents are pumped, which prevents deterioration of the transport equipment and enables a pumpless system.

[0071] Furthermore, the present invention can improve the efficiency of thermal energy through exhaust heat recovery and high-speed processing.

[0072] Furthermore, in the present invention, rapid cooling cracks can be prevented in response to thermal shocks that may occur when the same reactor is used for continuous intermittent production, thereby improving production efficiency.

[0073] Furthermore, in the present invention, the water vapor and sulfur components released from the production apparatus 1 can be eliminated by reducing the heat radiation loss during supply and by rapid cooling.

[0074] Furthermore, in the present invention, by increasing the amount of sulfur contained in the treatment agent, the amount of treatment agent used for the material to be treated can be reduced.

[0075] Furthermore, in the present invention, the safety of the reaction device 4 against an explosion or liquid leakage can be improved.

[0076] In addition, the treatment agent according to the present invention can also be used for difficult-to-react objects, such as objects that cannot be treated by two-stage treatment or yard aging, and objects that are not suitable for treatment by crushing treatment or pressurized / reduced pressure penetration treatment.

[0077] Furthermore, the treatment agent of the present invention can be easily used on-site depending on the object to be treated, for example, in combination with granular agents required for fast acting and long-term stability.

[0078] In addition, the sulfur particle size is small, and the sulfur can be easily used without using a special spreader or pump. [Explanation of symbols]

[0079] 1 Manufacturing equipment 2 Mixing equipment 3 Feeder 4 Reactor 5 Cooling device 6 Buffer device 7,8,9,10 Delivery pipes 11,12,13,14 Control valves 15 Compressor 16,17 Distribution pipe 18,19 Control valve 20,21,22 Supply pipe 23, 24, 25 Control valve 26 Supply pipe 27 Control valve 28 Water source 29 Cooling water flow path 30 Three-way valve 31 Exhaust stack

Claims

1. In an apparatus for manufacturing a treatment agent containing a polysulfide, a mixing device for mixing raw materials including sulfur, an alkaline compound, and water in a predetermined mixing ratio; a supply device for storing the raw materials mixed in the mixer and supplying them in predetermined amounts; a reactor for reacting the raw material supplied from the supply device at a predetermined pressure and a predetermined temperature to produce a treatment agent containing polysulfides; a cooling device for forcibly cooling the treatment agent produced in the reaction device to a predetermined temperature; a buffer device for allowing the treatment agent cooled by the cooling device to naturally dissipate heat up to a predetermined temperature and storing the treatment agent; having An apparatus for producing a polysulfide-containing treatment agent, characterized in that the raw materials and treatment agent are intermittently pumped between a supply device, a reaction device, and a cooling device to continuously produce a polysulfide-containing treatment agent.

2. 2. The apparatus for producing a treatment agent containing polysulfides according to claim 1, wherein the mixing device mixes sulfur, an alkaline compound, and water while crushing the sulfur and the alkaline compound under water.

3. 2. The apparatus for producing a polysulfide-containing treatment agent according to claim 1, wherein the reaction device produces the treatment agent by reacting sulfur, an alkaline compound, and water while crushing the sulfur and the alkaline compound underwater.

4. 2. The apparatus for producing a polysulfide-containing treating agent according to claim 1, wherein the reaction device pumps the treating agent to a cooling device using an increased pressure during the reaction.

5. The apparatus for producing a polysulfide-containing treatment agent according to claim 1, characterized in that the cooling device mixes a previously produced cooled treatment agent with a later produced uncooled treatment agent to cool them.

6. In a method for producing a treatment agent containing a polysulfide, a mixing device for mixing raw materials including sulfur, an alkaline compound, and water in a predetermined mixing ratio; a supply device for storing the raw materials mixed in the mixer and supplying them in predetermined amounts; a reactor for reacting the raw material supplied from the supply device at a predetermined pressure and a predetermined temperature to produce a treatment agent containing polysulfides; a cooling device for forcibly cooling the treatment agent produced in the reaction device to a predetermined temperature; a buffer device for allowing the treatment agent cooled by the cooling device to naturally dissipate heat up to a predetermined temperature and storing the treatment agent; Using a manufacturing device for a treatment agent comprising: A method for producing a polysulfide-containing treatment agent, comprising intermittently pumping raw materials and treatment agents between each device to continuously produce a polysulfide-containing treatment agent.

7. A method for producing a treatment agent containing polysulfides, comprising: treating sulfur and water, or sulfur, water and an alkaline compound, as raw materials in a reaction apparatus at a temperature below the melting point of sulfur, to produce a sulfur-containing substance; and adding the produced sulfur-containing substance to the treatment agent produced by the production method according to claim 6.

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