Method for preparing insoluble sulfur from crude sulfur

Abstract

The invention belongs to the technical field of coal chemical industry, and particularly relates to a method for preparing insoluble sulfur from coking crude sulfur. The invention provides a method for preparing insoluble sulfur from crude sulfur, which comprises the following steps of: 1, melting the crude sulfur, and settling to obtain sulfur liquid; 2, extracting the sulfur liquid by adopting an organic solvent under a microwave condition to obtain filtrate; 3, heating the filtrate, recovering the solvent, and adding a stabilizer to obtain liquid sulfur; 4, immersing the liquid sulfur into quenching liquid to obtain solid sulfur; and 5, mixing and separating the sulfur and the mixed solvent to obtain the insoluble sulfur. By adopting a microwave heating mode, energy can be preferentially concentrated to heat an organic solvent, so that the organic solvent is rapidly heated to dissolve sulfur; and the microwave technology is fast in extraction, so that the dissolution of tar can be reduced while sulfur dissolution is ensured, and the crude sulfur is purified. And heating the filtered filtrate to recover the organic solvent, quenching to obtain the insoluble sulfur, and separating and purifying by using a mixed solvent to obtain the insoluble sulfur.

Description

Technical Field

[0001] The invention belongs to the technical field of coal chemical industry, and particularly relates to a method for preparing insoluble sulfur from crude sulfur. Background Art

[0002] The crude sulfur, a byproduct of coke oven gas in a coking plant, is obtained in the desulfurization section of coke oven gas purification. The main production principle is to obtain elemental sulfur by catalytic oxidation of hydrogen sulfide in coke oven gas. Since coke oven gas contains a large amount of coal tar and dust, these substances will enter the crude sulfur, resulting in poor color of the crude sulfur, which is black or dark yellow. The sulfur content of crude sulfur is not high, generally 30-60% depending on production conditions, which limits the scope of use of crude sulfur as a byproduct of coking plants. Sometimes, due to poor color or low purity, it cannot be used and can only be piled up as solid waste. This has an adverse impact on the economic benefits and ecological environment of coking enterprises.

[0003] In order to solve the environmental problems caused by the crude sulfur produced as a byproduct of the coking plant and improve the economic benefits of the coking plant, the crude sulfur produced by the coking plant is now processed and made into high value-added insoluble sulfur. Insoluble sulfur is mainly used as a high-grade accelerator and vulcanizer in the rubber industry and is widely used in the production and manufacturing of tires and other rubber composite products, such as tire carcass rubber, cushion rubber, white tire side rubber, and rubber and skeleton material bonding rubber for tire retreading, hoses, and tapes. It can also be used in rubber products such as cables, rubber rollers, oil seals, rubber shoes, and light-colored rubber products with large sulfur consumption. Because insoluble sulfur can make the meridian, steel wire and rubber more firmly adhered, it can effectively prevent the rubber from frost spraying and improve the heat resistance and wear resistance of the tire. Insoluble sulfur is an indispensable and important raw material in tire production.

[0004] At present, the purification methods used by coking enterprises mainly include melting method, solvent method and gasification method. However, the purity of sulfur prepared by the existing preparation method is relatively low, ranging from 50 to 90%. The existing sulfur preparation methods for insoluble sulfur mainly include melting method, gasification method, etc., but the yield of insoluble sulfur is low, only between 20 and 40%. Summary of the invention

[0005] In view of this, the present invention provides a method for preparing insoluble sulfur from crude sulfur. By purifying crude sulfur according to the method provided by the present invention, insoluble sulfur with high purity and high yield can be obtained.

[0006] In order to solve the above technical problems, the present invention provides a method for preparing insoluble sulfur from crude sulfur, comprising the following steps:

[0007] The crude sulfur is melted and then precipitated to obtain sulfur liquid.

[0008] extracting the sulfur liquid with an organic solvent under microwave conditions to obtain a filtrate;

[0009] Raising the temperature of the filtrate to recover the solvent and adding a stabilizer to obtain liquid sulfur;

[0010] immersing the liquid sulfur in a quenching liquid to obtain solid sulfur;

[0011] The sulfur is mixed with a mixed solvent and separated to obtain insoluble sulfur.

[0012] Preferably, before the melting, the process further comprises: crushing and screening the crude sulfur in sequence to obtain crude sulfur particles;

[0013] The average particle size of the coarse sulfur particles is 0.2-1 mm.

[0014] Preferably, the sedimentation treatment is to keep the mixture still at the melting temperature, and the still time is 3 to 12 hours.

[0015] Preferably, the microwave power is 500-1000 W, the heating temperature is 70-130° C., and the dissolution time is 5-20 min.

[0016] Preferably, the organic solvent includes one or more of tetralin, decalin, nitrobenzene, chlorobenzene, dinitrobenzene, benzyl alcohol, styrene, carbon disulfide, benzene, toluene, xylene, tetrachloroethylene and o-xylene.

[0017] Preferably, the organic solvent is a mixed solution of toluene, xylene and chlorobenzene, and the mass ratio of toluene, xylene and chlorobenzene is 1:1:1-15.

[0018] Preferably, it is characterized in that the mass ratio of the organic solvent to the crude sulfur is 1 to 20:1.

[0019] Preferably, the dissolution further includes solid-liquid separation, and the solid-liquid separation is performed under insulation conditions, and the insulation temperature is consistent with the dissolution temperature.

[0020] Preferably, after the solid-liquid separation, the process further comprises:

[0021] The liquid obtained by solid-liquid separation is heated to obtain sulfur liquid;

[0022] The sulfur liquid is kept warm for a period of time and then a stabilizer is added to perform rapid cooling to obtain the insoluble sulfur;

[0023] Preferably, the heating temperature is 170-350° C. The heat preservation time is 5-20 minutes.

[0024] Preferably, the stabilizer is KCl, KBr, KI, hexachloroparaxylene, etc. The amount of the stabilizer is 0.5%-10% of the mass of the sulfur liquid.

[0025] Preferably, the quenching liquid is deionized water, acidic aqueous solution, ice, carbon disulfide, carbon tetrachloride, chlorinated hydrocarbons, benzene, or toluene.

[0026] Preferably, the mixed reagent is a mixed solution of toluene, xylene, chlorobenzene, carbon disulfide and ethanol, and the mass ratio of toluene, xylene, chlorobenzene, carbon disulfide and ethanol is 1:1:1:1:1:1-15.

[0027] Preferably, the mixing and separation further comprises:

[0028] The liquid obtained by solid-liquid separation is distilled, washed and dried to obtain ordinary sulfur;

[0029] The solid obtained by solid-liquid separation is washed and dried to obtain the insoluble sulfur.

[0030] The present invention provides a method for preparing insoluble sulfur from crude sulfur, comprising the following steps: melting crude sulfur and then settling it to obtain sulfur liquid. Extracting the sulfur liquid with an organic solvent under microwave conditions to obtain a filtrate; heating the filtrate to recover the solvent and adding a stabilizer to obtain liquid sulfur; immersing the liquid sulfur in a quenching liquid to obtain solid sulfur; and mixing and separating the sulfur with a mixed solvent to obtain insoluble sulfur. The present invention melts crude sulfur and then sets it to remove part of the tar and most of the ash and impurities in the crude sulfur, thereby preliminarily improving the purity of the crude sulfur. The present invention adopts a microwave heating method, which can allow energy to be preferentially concentrated on heating the organic solvent, so that the sulfur is quickly dissolved in the organic solvent and the extraction efficiency is improved; at the same time, microwaves have a weaker thermal effect on the components in the crude sulfur, while ensuring the dissolution of sulfur, reducing the dissolution of tar in the organic solvent, thereby improving the purity of sulfur. By heating the purified sulfur and adding a stabilizer, the sulfur can be efficiently polymerized into insoluble sulfur and the solvent can be recovered. It can be seen from the results of the examples that crude sulfur can be prepared into insoluble sulfur according to the preparation method provided by the present invention. The purity of the prepared insoluble sulfur is 99.9182-99.9827%, and the yield is 48.8539-74.728. DETAILED DESCRIPTION

[0031] The present invention provides a method for preparing crude sulfur, comprising the following steps:

[0032] The crude sulfur is melted and then precipitated to obtain sulfur liquid.

[0033] extracting the sulfur liquid with an organic solvent under microwave conditions to obtain a filtrate;

[0034] Raising the temperature of the filtrate to recover the solvent and adding a stabilizer to obtain liquid sulfur;

[0035] immersing the liquid sulfur in a quenching liquid to obtain solid sulfur;

[0036] The sulfur is mixed with a mixed solvent and separated to obtain insoluble sulfur.

[0037] The present invention melts crude sulfur and then settles it to obtain sulfur liquid. In the present invention, the crude sulfur is preferably a by-product of a coking plant, and the mass percentage of tar in the crude sulfur to the total mass of impurities is preferably 30-80%, and more preferably 40-70%. In the present invention, the melting preferably also includes: crushing and screening the crude sulfur in sequence to obtain crude sulfur particles. The present invention has no special restrictions on the crushing, as long as the crude sulfur can be formed into small particles. In the present invention, the average particle size of the crude sulfur particles is preferably 0.2-1.0 mm, more preferably 0.3-0.8 mm, and most preferably 0.4-0.6 mm. The present invention has no special requirements for the screening, as long as the average particle size of the crude sulfur particles can reach the above range. The present invention limits the average particle size of the crude sulfur particles to the above range, which is conducive to increasing the melting efficiency of sulfur and improving the precipitation efficiency of impurities.

[0038] In the present invention, the melting temperature is preferably 120-150°C, more preferably 130-140°C. In the present invention, the sulfur liquid obtained by melting the crude sulfur at the above-defined temperature has a low viscosity and thus has good fluidity, which is convenient for the precipitation of impurities in the crude sulfur. If the melting temperature is higher than 150°C, the sulfur liquid will become viscous, which is not conducive to the precipitation of impurities in the crude sulfur. In the present invention, the impurities preferably include one or more of tar, ash and miscellaneous salts. The present invention has no special limitation on the melting method, and the conventional method in the art can be used. In an embodiment of the present invention, the melting is carried out in an electric heater.

[0039] In the present invention, the sedimentation treatment is preferably heat-insulated and left to stand at the melting temperature, and the standing time is preferably 3 to 12 hours, more preferably 8 to 12 hours. In the present invention, after the sedimentation treatment, it is preferably further included: solid-liquid separation of the system after the sedimentation treatment. The present invention has no special requirements for solid-liquid separation, and conventional methods in the art can be used. The present invention can precipitate most of the tar and inorganic salt impurities in the crude sulfur through sedimentation treatment, thereby removing them and preliminarily improving the purity of the sulfur.

[0040] In the present invention, the power of the microwave is preferably 500-1000W, more preferably 700-800W; the frequency of the microwave is preferably 2000-3000Hz, more preferably 2450-2800MHz. In the present invention, the extraction time is preferably 5-20min, more preferably 10-15min; the extraction temperature is preferably 80-110°C, more preferably 80-105°C, and most preferably 90-100°C. In the present invention, the dissolution temperature is ensured by microwaves. In the present invention, the dissolution pressure is preferably normal pressure, and the pressure of the normal pressure is preferably 0.1MPa. The use of microwave heating technology can preferentially heat the solvent, while crude sulfur is non-polar and will not be heated under microwaves, and microwave heating takes less time than conventional heat transfer heating, which reduces the dissolution of other impurities in the organic solvent.

[0041] The present invention adopts an organic solvent to dissolve the sulfur liquid to obtain a sulfur-containing filtrate. In the present invention, the organic solvent preferably includes one or more of tetralin, decalin, nitrobenzene, chlorobenzene, dinitrobenzene, benzyl alcohol, styrene, carbon disulfide, benzene, toluene, xylene, tetrachloroethylene and o-xylene. More preferably, it is one or more of toluene, xylene and chlorobenzene, and most preferably, it is toluene, xylene and chlorobenzene. In the present invention, when the organic solvent is two or more of the above-mentioned specific substances, the present invention has no special requirements for the mass ratio of the specific substances, and any ratio can be used. In the present invention, when the organic solvent is toluene, xylene and chlorobenzene, the mass ratio of toluene, xylene and tetralin is preferably 1:1:1-15, more preferably 1:1:4-9, and further preferably 1:1:5-8. In the present invention, the mixed solution of toluene, xylene and chlorobenzene has a large solubility for sulfur, but hardly dissolves tar. At the same time, the mixed solution has a strong ability to absorb microwaves and is more easily heated in a microwave atmosphere. Using the mixed solution of toluene, xylene and chlorobenzene as an organic solvent to dissolve sulfur in crude sulfur can increase the sulfur dissolution rate and reduce the impurity dissolution rate, thereby greatly improving the purity of sulfur.

[0042] In the present invention, the mass ratio of the organic solvent to crude sulfur is preferably 1 to 20:1, more preferably 5 to 15:1, and further preferably 6 to 10:1.

[0043] In the present invention, the dielectric constant of crude sulfur is 2.7, which means that the coupling ability of non-polar substances to microwaves is extremely weak; generally speaking, a medium with a large dielectric constant is easy to be heated by microwaves, while a medium with a small dielectric constant is difficult to be heated by microwaves. The present invention performs extraction under the condition of microwave heating, which can ensure that microwave radiation can quickly heat the organic solvent with a large dielectric constant, and then the electromagnetic field generated by the microwave accelerates the diffusion of sulfur into the solvent, thereby increasing the solubility of sulfur in the solvent.

[0044] Microwave heating technology is a technology that heats materials based on the principle that the absorption of microwave energy by materials is the result of the interaction between polar molecules in the materials and the microwave electromagnetic field. Under the action of an external alternating electromagnetic field, the polar molecules in the materials are polarized and their orientations change with the change of polarity of the external alternating electromagnetic field. Such a large number of polar molecules frequently lose each other due to friction, so that electromagnetic energy is converted into heat energy. Usually, if you want to speed up the heating speed, you have to increase the heating temperature, but it is easy to cause the outside of the heated material to burn and the inside to not heat up. Microwaves can penetrate the inside of an object, and the heating process is carried out simultaneously in the entire object, with rapid heating, uniform temperature, and small temperature gradient. It is a "body heat source" that greatly shortens the heat conduction time in conventional heating.

[0045] In the present invention, the dissolution preferably further includes solid-liquid separation, and the solid-liquid separation is preferably performed under heat preservation conditions. In the present invention, the temperature of the heat preservation is preferably consistent with the temperature of extraction. In the present invention, the solid-liquid separation is preferably heat preservation filtration. The present invention has no special restrictions on the method of heat preservation filtration, and the conventional methods in the art can be used. In an embodiment of the present invention, the heat preservation filtration is preferably suction filtration.

[0046] The obtained filtrate is rapidly heated to 170-350°C, preferably 190-300°C, more preferably 200-220°C by microwave heating. The solvent is recovered during the heating process, and the sulfur ring is depolymerized to form a high molecular weight insoluble sulfur. After keeping the temperature for a period of time, a stabilizer is added. The stabilizer will be coupled with the free electrons at the chain end of the insoluble sulfur chain, block the chain end, and prevent depolymerization, so that linear long-chain molecules with different molecular weight distributions are obtained. The long-chain molecules are insoluble sulfur. The stabilizer used is KCl, KBr, KI, hexachloroparaxylene, and more preferably KCl. The amount used is 0.5-10%, preferably 2-8%, and more preferably 3-5%.

[0047] The polymerized sulfur liquid is quickly immersed in a quenching liquid, and the function of the quenching liquid is to quickly cool the insoluble sulfur to maintain the chain structure. If the temperature is naturally cooled, the chain-like insoluble sulfur will break and be reduced to a sulfur ring again, resulting in a decrease in the yield of insoluble sulfur. The quenching liquid is deionized water, acidic aqueous solution, ice, carbon disulfide, carbon tetrachloride, chlorinated hydrocarbons, benzene, and toluene.

[0048] Because all the sulfur cannot be completely polymerized into insoluble sulfur at the polymerization temperature, the obtained solid sulfur contains insoluble sulfur and ordinary sulfur. The insoluble sulfur is insoluble in organic reagents and can be separated by mixing. At the same time, the sulfur also contains a very small amount of impurities that can be washed with a mixed solvent. The solid sulfur remaining after separation and washing is insoluble sulfur, and the filtrate is ordinary sulfur after distillation.

[0049] The mixed reagent is a mixed solution of toluene, xylene, chlorobenzene, carbon disulfide and ethanol, and the mass ratio of toluene, xylene, chlorobenzene, carbon disulfide and ethanol is 1:1:1:1:1:1 to 13, preferably 1:1:1:1:1:1 to 15, and more preferably 1:1:1:1:1:1 to 8.

[0050] In the present invention, the mixing and separation preferably further comprises:

[0051] The liquid obtained by solid-liquid separation is distilled, washed and dried to obtain ordinary sulfur;

[0052] The solid obtained by solid-liquid separation is washed and dried to obtain the insoluble sulfur.

[0053] After obtaining the two solids, the present invention washes and dries the solids respectively to obtain the insoluble sulfur and ordinary sulfur. In the present invention, the washing solvent preferably includes ethyl acetate, ethanol, chloroform or quinoline, more preferably ethanol or chloroform. In the present invention, the ethanol is preferably anhydrous ethanol. In the present invention, the number of washings is preferably 2 to 5 times, more preferably 3 to 4 times. In the present invention, the drying is preferably oven drying, and the oven drying temperature is preferably 50 to 80°C, more preferably 55 to 75°C; the oven drying time is preferably 3 to 12 hours, more preferably 6 to 12 hours.

[0054] In order to further illustrate the present invention, the technical solutions provided by the present invention are described in detail below in conjunction with embodiments, but they should not be construed as limiting the protection scope of the present invention.

[0055] Example 1

[0056] The crude sulfur produced as a byproduct of the Liuzhou Iron and Steel Coking Plant is used as the preparation object, wherein the sulfur content of the crude sulfur is 70%, and the tar content of the crude sulfur is 14%;

[0057] The crude sulfur is crushed and sieved in sequence to obtain crude sulfur particles with an average particle size of 0.4 mm;

[0058] 200 g of crude sulfur particles were placed in an electric heater, heated to 130°C for melting, and then kept at this temperature for 8 hours for sedimentation treatment, and the supernatant was collected;

[0059] At a pressure of 0.1 MPa, a frequency of 2450 MHz, and a power of 700 W, a mixture of supernatant and organic solvent (a mixed solvent of toluene, xylene, and chlorobenzene in a mass ratio of 1:1:7) was added for microwave extraction; the mass ratio of the organic solvent to the supernatant was 8:1; the extraction time was 10 min, and the mixture was filtered with heat preservation;

[0060] The filtrate obtained by filtration was heated to 200°C by microwave to recover the solvent and kept warm for 10 minutes. Then, 2% by mass of potassium chloride stabilizer of liquid sulfur was added to react for 10 minutes and then quickly poured into 25°C deionized water for rapid cooling.

[0061] The quenched sulfur and the mixed solvent were mixed and stirred for 10 minutes, filtered, and the filtrate was distilled to obtain common sulfur; the solid left after filtering was insoluble sulfur. The solid was washed with ethanol for 3 times and then dried at 30°C for 3 hours to obtain insoluble sulfur and common sulfur respectively.

[0062] Embodiments 2 to 12

[0063] The preparation was carried out according to the method of Example 1, except for the differences shown in Table 1.

[0064]

[0065]

[0066] The sulfur dissolution rate and the sulfur retention rate of Examples 1 to 13 and Comparative Examples 1 to 4 were calculated according to Formula 1 and Formula 2, and the results are listed in Table 2.

[0067] Yield = S1 / S0×100% Formula 1;

[0068] Wherein, S0 is the mass of sulfur in crude sulfur / g, and S1 is the mass of insoluble sulfur / mass of ordinary sulfur / g.

[0069] The purity and yield of the sulfur obtained in Examples 1 to 13 were tested in the following manner:

[0070] Detection principle: Sulfur and sodium sulfite solution are heated and boiled together to convert into sodium thiosulfate, which is titrated with iodine standard titration solution, and the excess sodium sulfite is masked with formaldehyde; the reaction equations are shown in equations 3 to 5:

[0071] S+Na2SO3=Na2S3O3 Formula 3;

[0072] I2+2Na2SO3=Na2S4O6+2NaI Formula 4;

[0073] HCHO+Na2SO3+H2O=H2C(OH)SO3Na+NaOH Formula 5.

[0074] Detection steps: weigh the mass of the sample to be tested (accurate to 0.0001g) and place it in a 250mL conical flask, moisten it with 25mL anhydrous ethanol, add 50mL water and 5g anhydrous sodium sulfite, put a short-necked funnel on the bottle mouth, heat to boiling, keep a slightly boiling state until the sulfur is completely dissolved, and shake the conical flask from time to time during heating. Remove the conical flask, cool to room temperature, move to a 250mL volumetric flask, dilute to 250mL with water, shake up, and filter if necessary. Accurately draw 50mL of filtrate and place it in a 250mL conical flask, add 7mL of formaldehyde (GB685) solution with a mass concentration of 40%, place it for 3-5min, add 2 drops of phenolphthalein indicator with a mass concentration of 5g / L, use a 20% glacial acetic acid solution with a volume percentage until the red color disappears and an excess of 4-5 drops, add 3mL of starch indicator, and titrate with a molar concentration of 0.1mol / L iodine standard titration solution until the blue color appears as the end point.

[0075] The sulfur purity is calculated according to Formula 6 and the results are listed in Table 2:

[0076]

[0077] Wherein, C is the reagent concentration of the iodine standard titration solution, mol / L; V1 is the volume of the iodine standard titration solution consumed when titrating the sample, mL; V2 is the volume of the iodine standard titration solution consumed when titrating the blank, mL; m1 is the mass of the sample, g; m2 is the mass of the blank sample, g; 0.03207 is the mass of the blank sample with 1.00 mL of iodine standard titration solution. Equivalent mass of sulfur, g.

[0078] Table 2 Yield and purity of insoluble sulfur and common sulfur obtained in Examples 1 to 12

[0079]

[0080] Although the above embodiment describes the present invention in detail, it is only a part of the embodiments of the present invention, not all of the embodiments. People can also obtain other embodiments based on this embodiment without creativity, and these embodiments all fall within the protection scope of the present invention.

Claims

1. A method for preparing insoluble sulfur, comprising the following steps: The crude sulfur is melted and then precipitated to obtain sulfur liquid. extracting the sulfur liquid with an organic solvent under microwave conditions to obtain a filtrate; Raising the temperature of the filtrate to recover the solvent and adding a stabilizer to obtain liquid sulfur; immersing the liquid sulfur in a quenching liquid to obtain solid sulfur; The sulfur is mixed with a mixed solvent and separated to obtain insoluble sulfur.

2. The preparation method according to claim 1, characterized in that: Before the melting, the process further comprises: crushing and screening the crude sulfur in sequence to obtain crude sulfur particles; The average particle size of the coarse sulfur particles is 0.2-1 mm.

3. The preparation method according to claim 1, characterized in that: The sedimentation treatment is to keep the mixture still at the melting temperature, and the still time is 3 to 12 hours.

4. The preparation method according to claim 1, characterized in that: The power of the microwave is 500-1000 W, the heating temperature is 70-130° C., and the dissolution time is 5-20 min.

5. The preparation method according to claim 1, characterized in that: The organic solvent includes one or more of tetralin, decalin, nitrobenzene, chlorobenzene, dinitrobenzene, benzyl alcohol, styrene, carbon disulfide, benzene, toluene, xylene, tetrachloroethylene and o-xylene.

6. The preparation method according to claim 5, characterized in that: The organic solvent is a mixed liquid of toluene, xylene and chlorobenzene, and the mass ratio of toluene, xylene and chlorobenzene is 1:1:1-15.

7. The preparation method according to claim 1, 5 or 6, characterized in that: The mass ratio of the organic solvent to the crude sulfur is 1 to 20:

1.

8. The preparation method according to claim 1, characterized in that: The dissolution further includes solid-liquid separation, and the solid-liquid separation is carried out under heat preservation conditions, and the heat preservation temperature is consistent with the dissolution temperature.

9. The purification method according to claim 8, characterized in that: After the solid-liquid separation, the following steps are further included: The liquid obtained by solid-liquid separation is heated to obtain sulfur liquid; The sulfur liquid is kept warm for a period of time and then a stabilizer is added for rapid cooling to obtain the insoluble sulfur.

10. The preparation method according to claim 9, characterized in that: The heating temperature is 170-350° C. The heat preservation time is 5-20 minutes.

11. The preparation method according to claim 9, characterized in that: The stabilizer is KCl, KBr, KI, hexachloro-p-xylene, etc. The amount of the stabilizer is 0.5%-10% of the mass of the sulfur liquid.

12. The preparation method according to claim 9, characterized in that: The quenching liquid is deionized water, acidic aqueous solution, ice, carbon disulfide, carbon tetrachloride, chlorinated hydrocarbons, benzene, or toluene.

13. The preparation method according to claim 1, characterized in that: The mixed reagent is a mixed liquid of toluene, xylene, chlorobenzene, carbon disulfide and ethanol, and the mass ratio of toluene, xylene, chlorobenzene, carbon disulfide and ethanol is 1:1:1:1:1:1-15.

14. The purification method according to claim 13, characterized in that: The mixed separation further comprises: The liquid obtained by solid-liquid separation is distilled, washed and dried to obtain ordinary sulfur; The solid obtained by solid-liquid separation is washed and dried to obtain the insoluble sulfur.

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