CN117658078A - Method for preparing particle diameter sulfur powder by using microreactor and product thereof - Google Patents

Abstract

The invention relates to a method for preparing particle diameter sulfur powder by using a microreactor and a product thereof, wherein the method comprises the following steps: introducing liquid sulfur and water into the microreactor respectively, and cooling, filtering and drying the mixture discharged from the outlet of the reaction product of the microreactor to obtain the particle diameter sulfur. The invention prepares the micro-particle diameter sulfur through the micro-reactor, realizes that the particle diameter range of the sulfur can be mostly less than 45 microns, and has no other waste except water which can be recycled in the preparation process.

Description

Method for preparing particle diameter sulfur powder by using microreactor and product thereof

Technical Field

The invention belongs to the field of elemental sulfur powder preparation, and particularly relates to a method for preparing small-particle-diameter sulfur powder by using a microreactor and a product thereof.

Background

Sulphur for agricultural applications is generally in the form of flakes or granules, typically from 1mm to 10mm in size, and smaller particle sizes are required to prepare sulphur into agricultural formulations, for example, pesticide suspensions, wettable powders and the like typically require particle sizes of less than 10 microns, with an average particle size of about 5 microns. For industrial application of sulfur, namely, sulfur is used as a solid industrial raw material, the sulfur is generally required to be crushed, and the crushed sulfur is easier to add and disperse in industrial products.

The existing granulation molding technology of elemental sulfur mainly comprises air granulation, water granulation, steel belt granulation, roller granulation and other methods. The liquid sulfur is solidified into granular products, the size of the granular products is generally 1-6mm, and the granular products are characterized in that the granular sulfur has less dust and is not easy to break, and the mechanical flow production is convenient to carry out in the processes of loading, transporting and storing.

The preparation method mainly comprises the steps of sheeting forming and steel belt granulating, wherein the flaky sulfur prepared by the sheeting forming is irregular in shape and poor in appearance quality, a large amount of dust can be generated in the circulation process, and the packaging, loading and unloading and transportation costs are high. The forming of the knot piece mainly comprises the following steps: (1) The drum flaking is that the drum is cooled by water and is partially immersed in liquid sulfur, the liquid sulfur immersed on the surface of the drum rotates along with the drum, a layer of solid thin sulfur is formed by cooling after the liquid level is exposed, and the flaked sulfur is obtained by scraping by a scraper. The drum forming machine is convenient to operate, but has limited processing capacity, and is suitable for small-scale production. The prior natural gas treatment plant in Chuan Yu area still uses the process because of low sulfur yield; (2) The belt type flaking, namely the liquid sulfur slowly flows onto the steel belt, cold water is sprayed on the back of the steel belt to cool and solidify the liquid sulfur rapidly, the steel belt is more complex than a drum flaking machine, the occupied area is large, the requirements on the steel belt materials are strict, the steel belt flaking is suitable for large and medium-sized devices, the thickness of the produced flaky sulfur product is 5-7mm, the width is 5-10mm, the water content is less than 1%, and the bulk density is 1200kg/m ³ . The flaking process has poor product shape, is easy to crush, and the generated dust is easy to cause potential safety hazard and environmental pollution in the processes of packaging, transportation and use by users, so that the equipment maintenance workload is large, and the equipment maintenance workload is large in ChinaGranular sulfur is required by large households using sulfur, so that a flaking process is not suitable for a natural gas purification plant with high sulfur content.

The steel belt granulating process has good product quality and intermittent operation, is very suitable for the production scale of refineries, and is the most commonly adopted method by large-scale sulfur manufacturers. At present, the sulfur granulation process mainly comprises the following steps: the air granulation process comprises the following steps: air with constant temperature of about 30 ℃ is blown into a conical granulating tower from the tower bottom, liquid sulfur is sprayed in the tower bottom, mist sulfur is formed in high-speed air flow, particle sulfur is formed by aggregation, the sulfur particles are obtained through extraction and screening, the water content is less than 0.5%, the bulk density is 1100kg/m < 3 >, the brittleness is less than 1.0%, and the repose angle is less than 25 degrees. (2) Water granulation process. Liquid sulfur is sprayed into the stainless steel granulating tank from a top nozzle, and meanwhile, cooling water containing surfactant is pumped into the tank along the tank wall. The liquid sulfur is cooled into spherical particles in water, discharged from the bottom of the tower together with cooling water, and subjected to sieving and dehydration to obtain a solid sulfur particle product. The sulfur granule has a water content of about 2.0% and a bulk density of 1070kg/m between 1-6mm ³ The brittleness is less than 3.0 percent, and the repose angle is less than 32 degrees. (3) The steel belt granulating process includes the steps of uniformly dropping liquid sulfur onto steel belt moving at uniform speed through a distributor, and arranging a continuous spray water cooling device below the steel belt to cool and solidify materials on the steel belt rapidly during moving to form granules. The steel belt granulated sulfur product is a superior product, the diameter of the hemispherical grain is between 1 and 6mm, the water content is less than 0.5%, the bulk density is 1080kg/m < 3 >, the brittleness is less than 1.0%, and the repose angle is 30 degrees. (4) The roller granulating process, also called rotary granulating process or coarse grain making process, in which liquid sulfur is sprayed and coated on the surface of flowing small particle sulfur and cooled and solidified by air to make the particles grow up. And repeating the steps to form the sulfur product with the diameter of 1-6 mm. The diameter of the roller molding product is 1-6mm, the water content is 0.5%, the bulk density is 1220kg/m3, the brittleness is less than 1.0%, and the repose angle is 27 degrees.

In the prior patents, a number of sulphur particle production processes are also disclosed, for example WO1998038126A1 discloses a process for producing sulphur particles by heating sulphur until it melts, adjusting the temperature of the water and inducing the water to move at a certain velocity, injecting an uninterrupted stream of molten sulphur under pressure into the water moving at a certain velocity, the molten sulphur being explosively dispersed into fine sulphur particles, the shearing force generated by the movement of hot water at a certain velocity enhancing the explosive dispersion of molten sulphur. For example, US patent 4364774 discloses a method of granulating sulfur to make it easier to handle, comprising pouring an uninterrupted stream of molten sulfur into a water bath, and obtaining the granules by a milling process. Also, U.S. patent No. 4043717 discloses an apparatus for producing particulate sulfur from a molten sulfur stream. The apparatus has a spray head surrounded by an annular water jacket, and impingement of water onto the molten sulfur results in the formation of so-called "irregular particulate pellets" of sulfur. The device does not produce particles of uniform size. Canadian patent CA1151372 discloses a process for granulating sulfur by solidifying sulfur droplets in a countercurrent gas stream, in particular by introducing liquid sulfur into a vertical gas stream having a downwardly increasing linear velocity, and as an additional cooling medium, water may be introduced into the gas stream in the form of a mist. Canadian patent CA1314671 discloses a method of solidifying sulfur into particles by directing jets of water and sulfur onto a rotating disk. The sulfur hardens onto the disk and becomes particulate as a result of water impingement. The water and sulfur are then spun off the rotating disk. EP2406176B1 discloses a process for producing micronized sulphur powder products and micronized sulphur cake intermediates. The preparation of micronized sulphur emulsion from molten sulphur and dispersant solution, followed by removal of the dispersant solution, yields a good quality product, and the production process itself has enhanced safety and economic attributes. US20130230448A1 discloses a process for producing micronized sulphur in which elemental sulphur is dissolved in a solvent for sulphur to produce a sulphur solvent solution and precipitation of the dissolved sulphur is effected or controlled by manipulating at least one of pressure, temperature or water content in the solvent to produce micronized sulphur. Chinese patent CN112079335a discloses a method for preparing nano elemental sulfur particles, comprising the steps of: dissolving a solid sulfur source in an organic solvent, and filtering impurities possibly contained to prepare a sulfur-containing solution A; dissolving a surfactant in a second solvent to prepare a solution B; adding the sulfur-containing solution A and the sulfur-containing solution B into a micro-channel reactor or a hypergravity rotating packed bed respectively from a feed inlet, fully mixing feed liquid, and collecting slurry containing sulfur nano particles from a discharge outlet; drying the slurry containing the sulfur nano particles to remove the solvent, thereby obtaining nano elemental sulfur powder.

The preparation method of the sulfur particles disclosed by the invention is complex in process or waste is generated in the process, and the novel preparation method of the sulfur particles is provided, so that the prepared sulfur particles are more beneficial to industrial application and agricultural application, and the production process is simple, the process is free of waste, and the environment-friendly and efficient.

Disclosure of Invention

In order to solve the technical problems, the invention provides a method for preparing sulfur with micro particle size, which is characterized by comprising the following steps: and respectively introducing liquid sulfur and water or inert gas into the microreactor, and cooling, filtering and drying a mixture discharged from a reaction product outlet of the microreactor to obtain the particle diameter sulfur.

In the method, the liquid sulfur is prepared by heating, and generally the liquid sulfur is required to contain a trace amount of solid impurities, namely, after the sulfur is melted (namely, the liquid sulfur is melted), particles which are not melted or a small amount of microparticles are smaller than 45 microns in particle size, so that the protection of a microreactor is ensured, and the quality of the liquid sulfur after being subjected to the micronization is also ensured.

In the above-described method, the microreactor is also referred to as a microchannel reactor, and a conventional mixing microreactor can be applied to the above-described method of the present invention. Preferably, the microreactors have a microchannel size of between 10 and 2000 microns. Preferably, the cross-sectional area of the channels in the microreactor is from 100 to 4000000 square micrometers, preferably the cross-sectional area of the fluid channels is from 100 to 100000 square micrometers, and the total volume of the channels is from 10 to 500ml.

Preferably, in the above method, the cooling is performed by spraying the mixture discharged from the outlet of the reaction product of the microreactor into the aqueous solution or cooling the surface of the aqueous solution, that is, cooling water is used. The spray nozzle is in water, so that dust or aerosol cannot be generated, the cooling speed is high, the spray nozzle is blocked once the spray speed is reduced or the temperature is too low, stirring operation is partially affected by the spray nozzle in water, aerosol can enter the water through free falling, suspended solids of sulfur particles can be formed on the water surface through spraying, the suspended solids gradually sink into the water bottom through stirring, the operation is convenient, the problem of blockage of the spray nozzle cannot be caused, and a closed space is needed, so that the water mist generated by spraying is prevented from drifting to a production environment. The two methods have little influence on the particle size of the particles, and the particle size has no relation with the water injection or the water injection.

Preferably, in the above method, the cooling, filtering and drying method is to directly spray the mixture discharged from the outlet of the reaction product of the microreactor into a spray dryer by using a spray nozzle, and then discharge the gas in the spray dryer into a cyclone separator for cooling, so that the particulate sulfur is directly obtained without filtering and drying steps.

Preferably, in the above method, the mass ratio of the liquid sulfur to the aqueous solution is 1:0.5-20, preferably, the mass ratio of the liquid sulfur to the water is 1:0.5-10, and particularly preferably, the mass ratio of the liquid sulfur to the water is 1:4-9. The mass ratio of liquid sulfur to water can be changed within a certain range, and from the research result, the higher the proportion of water, the smaller the average particle diameter of the product, and the higher the mass ratio of sulfur particles with the particle diameter of less than 45 micrometers, but the larger the water quantity can affect the production, so that the maximum water consumption can be properly adjusted according to the two aspects of yield requirement and quality requirement, the maximum water consumption is 4 times of the mass of the sulfur at present, and the maximum water consumption can be adjusted to 3 times, even 2 times, even 1 time of the mass of the liquid sulfur if possible, but the average particle diameter of the sulfur is increased, but the production can be improved. This can be adjusted in the industrial production according to the quality and yield of the sulphur particles.

Preferably, in the above method, the temperature of the liquid sulfur and water is 90-200 ℃. Preferably, the temperature of the liquid sulfur is 110-170 ℃, preferably the temperature of the liquid sulfur is 120-150 ℃, particularly preferably the temperature of the liquid sulfur is 130-145 ℃, the temperature of the water is 0-200 ℃, preferably the temperature of the water is 90-200 ℃, particularly preferably the temperature of the water is 100-150 ℃. The temperature of the sulfur and the temperature of the water can be the same or different, but in order to realize the sufficient mixing and dispersion of the sulfur and the water in the microreactor, the temperatures are preferably controlled to be similar, preferably the same, so that the mass transfer and the heat transfer between the sulfur and the water can be reduced, the dispersion speed of the liquid sulfur and the water can be improved, and the liquid sulfur drop particles in the mixture sprayed from the outlet of the microreactor can be sufficiently and uniformly dispersed in the water. Of course, in order to achieve a smaller increase in the particle fraction, for example, a 25 μm or less sulphur particle fraction, the temperature may be increased higher, for example, to 200 ℃, and of course the higher the temperature the greater the energy consumption and the greater the equipment load. The temperature can be properly regulated according to production needs, and the temperature is regulated to 130-145 ℃ mainly for energy conservation, and the temperature can be increased under the condition of not considering energy conservation, such as for realizing smaller increase of the duty ratio of sulfur particles.

Preferably, in the above method, the pressure of the liquid sulfur and the water is 0.15-0.5MPa, preferably, the pressure of the liquid sulfur and the water is 0.2-0.5MPa, and the pressure of the liquid sulfur and the water may be the same or different, so that in order to enable the water to rapidly disperse the sulfur, the pressure of the water may be generally selected to be greater than the pressure of the sulfur, or the pressure of the sulfur may be greater than the pressure of the water, so as to improve the mixing efficiency of the liquid sulfur and the water in the microreactor. The pressure of the liquid sulfur and the water is directly conducted into the microreactor, so that the pressure of a reactant outlet of the microreactor is basically similar to the pressure of the liquid sulfur and the water, the pressure of an injection port is similar to the pressure of the liquid sulfur and the water, the greater the pressure is, the greater the pressure of the mixture of the liquid sulfur and the water is injected by the injection port, and the higher the yield per unit time is under the condition of the same caliber of the injection port, but the higher the pressure is, the higher the energy consumption is caused.

Preferably, in the above method, the water is an aqueous solution or steam. The dispersion effect of the liquid sulfur and the aqueous solution directly fed into the microreactor will be better than that of the water vapor, and the main expression is that the particle size of the sulfur particles of the product fed into the microreactor by the aqueous solution is smaller and mainly concentrated in 25-45 microns, while the sulfur particles prepared by the water vapor are mostly in the particle size range of 45-75 microns.

Preferably, in the above method, the inert gas is a gas that does not react with sulfur under the process conditions, and preferably, the inert gas is nitrogen.

Preferably, in the above method, the water circulation sleeve is used for recycling, that is, in the case of cooling the mixture sprayed from the outlet of the microreactor by using the aqueous solution, the cooled aqueous solution is subjected to solid-liquid separation, and the water circulation sleeve is fed into the microreactor, so that even if the sulfur particles which are not completely filtered exist in the water circulation sleeve, the dispersion of the liquid sulfur is not affected, and the sulfur particles contained in the water circulation sleeve are not wasted and can be obtained by filtering again.

The invention also provides the particle diameter sulfur powder prepared by the method, which is characterized in that the average particle diameter of the sulfur powder is 2-50 microns, preferably, the average particle diameter of the sulfur powder is 20-50 microns, preferably, the average particle diameter of the sulfur powder is 30-40 microns.

In the above sulfur powder, the method that the average particle diameter is a linear average diameter is used for measurement and calculation, that is, the diameters of all sulfur particles in the sulfur particle sample are added and then divided by the total number of the sulfur particles, and the average particle diameter of the sulfur particles is equal to the arithmetic average value of the diameters of all the particles.

Preferably, the mass ratio of the particle diameter of the sulfur powder is more than 80%, preferably, the mass ratio of the particle diameter of the sulfur powder is more than 80% -98%, particularly preferably, the mass ratio of the particle diameter of the sulfur powder is more than 85% -97%, and the mass ratio of the particle diameter of the sulfur powder is more than 2-45 micrometers.

Preferably, the sulfur powder is a fine particle diameter sulfur powder, the mass ratio of the particle diameter of the sulfur powder is more than 80%, preferably, the mass ratio of the particle diameter of the sulfur powder is more than 80% -98%, particularly preferably, the mass ratio of the particle diameter of the sulfur powder is more than 85% -97%, and the mass ratio of the particle diameter of the sulfur powder is more than 25-45%.

The beneficial effects of the invention are that

1. The invention prepares the micro-particle diameter sulfur through the micro-reactor, realizes that the particle diameter range of the sulfur can be mostly less than 45 microns, and has no other waste except water which can be recycled in the preparation process.

2. According to the invention, the research surface of the process for preparing sulfur by adopting the microreactor can realize the particle diameter of sulfur at 150 ℃, so that the particle diameter of sulfur powder is less than 45 microns, and no dust is generated in the process.

3. The invention solves the problems that the sulphur has difficult micro-particle diameter and dust or other pollutants are generated in the micro-particle diameter process for optimizing process conditions, particularly the mass ratio of liquid sulphur to water, the temperature of raw materials entering a micro-reactor and the like.

Detailed Description

The sulfur used in the following examples is flaky elemental sulfur, no insoluble impurities are detected in the elemental sulfur, the purity of the elemental sulfur is more than or equal to 99%, and the water content of the elemental sulfur is less than or equal to 1%.

The measurement of the particle size and the measurement of the duty ratio of different particle sizes are carried out by adopting a particle size analyzer.

The microreactors used in the examples below had a channel cross-sectional area of 1000000 square micrometers and a total microchannel area of 280 square millimeters.

1. Experimental method for preparing sulfur microparticles

(1) Preparation of sulphur microparticle preparation apparatus

Preparation device A: preparing a high-pressure reaction kettle, arranging a sulfur melting container and an aqueous solution container in the reaction kettle, connecting the sulfur melting container and a micro-reactor outside the high-pressure reaction kettle through a pipeline, arranging a sulfur valve on a pipeline before entering the micro-reactor (outside the reaction kettle), then connecting the pipeline to an inlet of the micro-reactor again, connecting the aqueous solution container to the micro-reactor outside the reaction kettle through the pipeline, arranging a hot water valve on the pipeline before entering the reactor (outside the reaction kettle), then connecting the pipeline to the inlet of the micro-reactor again, connecting an outlet of the micro-reactor to the pipeline, arranging a product output valve on the pipeline, then connecting an injection port again, and cooling a reaction product in aqueous solution through the injection port. A pressure test meter and a thermometer are arranged in the high-pressure reaction.

Preparation device B: preparing a high-pressure reaction kettle, arranging a sulfur melting container and an aqueous solution container in the reaction kettle, connecting the sulfur melting container and a microreactor outside the high-pressure reaction kettle through a pipeline, arranging a sulfur valve on a pipeline before entering the microreactor (outside the reaction kettle), then connecting the pipeline with an inlet of the microreactor, connecting the aqueous solution container with a heat-preserving vaporization container outside the reaction kettle through the pipeline, arranging a water vapor valve on the pipeline of the vaporization container, then connecting the pipeline with the inlet of the microreactor, connecting an outlet of the microreactor with the pipeline, arranging a product output valve on the pipeline, then connecting an injection port, and cooling a reaction product in aqueous solution through the injection port. A pressure test meter and a thermometer are arranged in the high-pressure reaction.

(2) 400g of sulfur is weighed into a 500ml sulfur melting container, water close to 5000g is added into an aqueous solution container, a high-pressure reaction kettle or an aqueous solution heating kettle is closed, and heating is started.

(3) A5000 ml container was prepared, the upper part of which was provided with an inlet and an outlet of the jet port and the lower part of which was put into an aqueous solution, and which was provided with a stirring paddle for stirring the liquid, and which served as a collector of the reaction product of the microreactor.

(4) When the pressure and the temperature in the high-pressure reaction kettle or the pressure and the temperature in the aqueous solution heating kettle reach the requirements, firstly opening and adjusting a sulfur valve, a hot water valve or a water vapor valve, then opening a product output valve, fully mixing molten sulfur and water in a micro-reaction to enable the sulfur to become tiny particles dispersed in the aqueous solution, forming a mixture of the molten sulfur particles and the aqueous solution, then spraying the mixture into water of a collector through the product output valve, and cooling in the water to obtain the mixture of the sulfur tiny particles and the water.

(5) Concentrating and drying the mixture of the sulfur microparticles and water to obtain powder of the sulfur microparticles.

Standing the mixture of the sulfur microparticles and the water for about 3 hours, and extracting supernatant after the sulfur microparticles are completely settled to obtain the mixture of the sulfur microparticles with the sulfur content of about 50 percent and the water; then pouring the mixture of the sulfur microparticles and water into a suction filtration bottle for suction filtration to obtain a wet sulfur microparticle product; and (3) putting the product into a 60 ℃ oven for drying to obtain a sulfur microparticle dry powder sample, and testing the particle size condition of sulfur particles of the powder.

2. Preparation example of Sulfur microparticles

Example 1: influence of the ratio of elemental sulfur mass to water mass entering the microreactor on particle size

And (3) heating sulfur and water to 130 ℃ simultaneously by adopting a preparation device A (the pressure value is 0.27 Mpa), adjusting a valve, injecting the sulfur and water into a solution through an injection port for outputting a product according to the mass ratio of the elemental sulfur and the water entering the microreactor of 5:95, 10:90, 15:85 and 20:80, cooling, filtering and drying, and carrying out particle size detection on a sulfur microparticle sample collected after the cooling, filtering and drying, wherein particle size detection data are shown in the following table 1.

TABLE 1 influence of elemental Sulfur and Water Mass ratio on the particle size of Sulfur microparticles

As can be seen from the above table data, the sulfur sample particle size becomes smaller with increasing water ratio, the sulfur particle fraction below 45 microns decreases, and the mass fraction of sulfur particles above 45 microns increases, which results in an increase in the average particle size. Wherein the particle size range is 0.025-0.045mm, 0.045-0.075mm, the data specifications in tables 2 and 3 below are the same as this.

Example 2: influence of elemental sulfur temperature and water temperature entering microreactor on particle size

The preparation device A is adopted, the ratio of the mass of elemental sulfur to the mass of water is 10:90, the heating temperature of sulfur and water is 130 ℃, 135 ℃, 140 ℃ and 145 ℃, the temperature of sulfur and water is the same, the sulfur and the water are sprayed into a solution through a spraying port for outputting products, and particle size detection is carried out on a sulfur microparticle sample collected after cooling, filtering and drying, wherein the detection data are shown in the following table 2:

table 2: data of influence of sulfur temperature and water temperature on particle size

As can be seen from the above table data, the sulfur sample particle size becomes smaller with increasing temperature of the sulfur and water entering the microreactor, but the particle duty cycle during the 25 to 45 microns is less influential, the primary effect being an increase in the duty cycle of particles smaller than 25 microns and a decrease in the duty cycle of particles larger than 75 microns.

Example 3: influence of Water vapor and liquid Water on Sulfur particles

The experiment was performed using preparation apparatus B with steam instead of aqueous solution. The reaction kettle is internally provided with a sulfur melting container and an aqueous solution container, the mass ratio of sulfur to water is 10:90, the heating temperature of the sulfur to water is 130 ℃, the temperature in the sulfur melting container is the same as the temperature of water vapor, a sulfur valve and a water vapor valve are simultaneously opened under the condition that the pressure in the vaporization container is the same as the pressure of the water vapor and are input into a micro-reactor, the micro-reactor is sprayed into a solution through a jet orifice of product output, and a prepared sulfur microparticle sample is collected for particle size detection after cooling, filtering and drying, wherein the average particle size is 45 mu m.

In order to verify whether the two cooling modes of injecting the mixture output by the microreactor into water through the injection port and injecting the mixture into the water surface can influence the particle size of sulfur, in the 3 experimental processes, the injection port is transferred into another cooling container in the middle part time (about 2 minutes), clean water is contained in the cooling container, the injection nozzle injects mist water vapor at the distance of about 5 cm above the water surface, the water vapor condenses on the surface of the water solution, then the particle size of sulfur particles is measured, and the particle size condition of the sulfur particles is equal to the particle size condition of sulfur injected in the corresponding water solution, namely, the above-water injection and below-water injection cooling are selected to have no influence on the particle size of the sulfur particles.

Claims (10)

1. A method for preparing sulfur with micro particle size, which is characterized in that the method comprises the following steps: and respectively introducing liquid sulfur and water or inert gas into the microreactor, and cooling, filtering and drying a mixture discharged from a reaction product outlet of the microreactor to obtain the particle diameter sulfur.

2. The method according to claim 1, wherein the cooling is performed by spraying the mixture discharged from the outlet of the reaction product of the microreactor into an aqueous solution or by cooling the surface of the aqueous solution.

3. The method of claim 1, wherein the cooling, filtering and drying is carried out by spraying the mixture discharged from the outlet of the reaction product of the microreactor directly into a spray dryer by using a spray nozzle, and then discharging the gas in the spray dryer into a cyclone separator for cooling, and the particulate sulfur is directly obtained without filtering and drying steps.

4. The method according to claim 1, characterized in that the mass ratio of the liquid sulphur to the aqueous solution is 1:0.5-10.

5. The method according to claim 1, characterized in that the temperature of the liquid sulphur is 110-170 ℃, preferably the temperature of the liquid sulphur is 120-150 ℃, the temperature of the water is 0-200 ℃, preferably the temperature of the water is 90-200 ℃.

6. The method according to claim 1, characterized in that the pressure of the liquid sulphur and water is 0.15-0.5MPa.

7. The method according to claim 1, wherein the water is an aqueous solution or steam and the inert gas is nitrogen.

8. A particulate sulphur powder prepared by the method of any one of claims 1 to 7, wherein the sulphur powder has an average particle size of from 2 to 50 microns, preferably from 20 to 50 microns.

9. The fine particle diameter sulfur powder according to claim 8, wherein the mass ratio of the particle diameter of the sulfur powder is 80% -98% in the range of 2 microns to 45 microns.

10. The fine particle diameter sulfur powder according to claim 8, wherein the mass ratio of the particle diameter of the sulfur powder is 85% -97% in the range of 2 micrometers to 45 micrometers.