Patent Description:
With the rapid increase of oil consumption, the global oil resources are scarcer increasingly, and the raw materials in refineries are heavier and poorer increasingly; at the same time, the environmental protection laws and regulations in different countries become stricter increasingly, and the control on the total sulfur content in petroleum products and natural gas become stricter increasingly. Therefore, the capacities of sulfur recovery units in major refineries and natural gas purification plants are increased rapidly. The domestic and international markets of common sulfur have become saturated, and the price of common sulfur is lower increasingly. How to provide high value-added sulfur products that are in short supply in the markets has become a focus of interest of relevant enterprises.

Insoluble sulfur is a high-efficiency rubber vulcanizing agent, which has the advantages of high distribution stability in rubber compounds, uniform vulcanization cross-linking points of vulcanization in products, etc., and can avoid frosting on the surfaces of rubber compounds and improve the adhesion between rubber and steel wires or chemical fiber cords.

The patent application No. <CIT> has disclosed an insoluble sulfur production method, which comprises the following steps: (<NUM>) melt polymerization; (<NUM>) atomization and cold extraction; (<NUM>) curing; (<NUM>) centrifugal separation; (<NUM>) continuous drying; (<NUM>) crushing, screening and oil filling, so as to obtain a finished product finally; although the method is a continuous production method, the required sulfur polymerization temperature and pressure are high with the method, specifically, the operating temperature is <NUM>-<NUM>, and the operating pressure is <NUM>-<NUM>. 2MPa; therefore, the requirements for the reaction apparatus are high.

The patent application No. <CIT> has disclosed heat-resistant and stable insoluble sulfur and a production method thereof. The production method comprises: (<NUM>) pre-melting: loading industrial raw sulfur into a sulfur melting pool at <NUM>-<NUM> and pre-melting, till the raw sulfur is turned into liquid sulfur; (<NUM>) reaction: introducing the liquid sulfur into a reaction kettle, adjusting the temperature to <NUM>, adding <NUM>% KI, and keeping the reaction for certain time under the conditions of N<NUM> shielding and mechanical stirring; (<NUM>) quenching: loading the product obtained in the step (<NUM>) in a gasification chamber containing N<NUM> for gasification to form superheated vapor, and spraying the superheated vapor into quenching water for quenching; (<NUM>) extraction: extracting the sulfur in the quenching water with an organic solvent; (<NUM>) crushing: loading the extracted sulfur into a dryer at <NUM>-<NUM> and carrying out drying till the moisture content in the sulfur is reduced to <NUM>%-<NUM>% of the moisture content before drying, then crushing the sulfur in a tube mill, and screening the crushed suffer through a <NUM>-400mpi sieve, so as to obtain heat-resistant and stable insoluble sulfur.

The properties of the insoluble sulfur obtained through extruding and quenching, gas drying and curing, and mechanical crushing procedures, etc. with the existing low-temperature melting method are unsatisfactory. During the discharging and quenching of the polymerized sulfur, the polymerized sulfur is usually discharged by extrusion into a quenching tower for quenching. Thus, the quenched material is in the form of lumps, which are not easy to transport because they may cause clogging in the pipeline and equipment. Therefore, the lumps can only be transported intermittently among different devices or apparatuses, resulting in a complex system operation process.

<CIT> relates to a production process for preparing insoluble sulphur through a low temperature method, wherein industrial sulphur is adopted as a raw material, heating liquefaction, polymerization reaction, quenching, drying, crushing, extraction and oil filling are sequentially performed, the polymerization reaction is performed at a temperature of <NUM>-<NUM>, and stabilizers are respectively added during the polymerization reaction stage, the quenching stage, and the oil filling stage.

<CIT> relates to heat-resistant stable non-soluble sulfur and a production method thereof. The production method comprises the steps of premelting; reaction; quenching; extraction; and smashing.

<CIT> relates to a production process for preparing insoluble sulfur high in thermal stability and content. Common industrial sulfur is adopted as a raw material, sulfur melting, a polymerization reaction, atomizing quenching, extracting, drying, smashing, purifying, screening and oil charging are sequentially conducted.

To solve the problems of a complex intermittent operation process and poor product properties in the production of insoluble sulfur through a low-temperature melting process in the prior art, the present invention aims at providing an insoluble sulfur production system and a method thereof, which solve the problems of difficult solid material transportation and poor product properties, and can be used to obtain insoluble sulfur with high product purity, high thermal stability, and high yield.

In an aspect, the present invention provides an insoluble sulfur production system, which comprises a polymeric kettle having a first discharge port and a quenching tower having a feed port, wherein the first discharge port is in communication with the feed port, and the quenching tower comprises a cylindrical housing, a granulation device and a shear pump, the housing comprises a feed quenching section and a discharging section that are arranged from top to bottom, and the side wall of the housing is provided with a solvent inlet for providing a solvent and a quenching agent inlet for providing a quenchant, wherein:.

In another aspect, the present invention provides an insoluble sulfur production method, which comprises:.

With the above technical scheme, the insoluble sulfur production system provided by the present invention can accomplish granulation, quenching, curing extraction, and crushing extraction in the quenching tower and output a slurry material. By granulation in the granulation device after the feeding, it can ensure that the material is in a granular state in the follow-up quenching, curing and extraction process, so that the material contacts with the solvent and the quenchant extensively and can form a circulating flow along with the liquid; the shear pump and the filter screen ensure that the slurry material can be outputted from the second discharge port, thus avoiding clogging in the transportation pipeline during subsequent transportation; the granulation device, circulating pump, shear pump, inner circulating cylinder and liquid distributor etc. can realize uniform distribution of the temperature field during material quenching, as well as integrated operation of curing extraction and crushing extraction.

<NUM> - polymeric kettle; <NUM> - quenching tower; <NUM> - housing; <NUM> - feed quenching section; <NUM> - material circulation section; <NUM> - discharging section; <NUM> - solvent inlet; <NUM> - quenching agent inlet; <NUM> - material separation section; <NUM> - circulating liquid outlet; <NUM> - material flow guide plate; <NUM> - granulation device; <NUM> - first feed pipe; <NUM> - first distribution pipe; <NUM> - first fixed pipe; <NUM> - first rotary pipe; <NUM> - first discharge channel; <NUM> - first discharge hole; <NUM> - shear pump; <NUM> - inner circulating cylinder; <NUM> - circulating flow guide plate; <NUM> - liquid distributor; <NUM> - filter screen; <NUM> - quenchant distributor; <NUM> - second feed pipe; <NUM> - second distribution pipe; <NUM> - second fixed pipe; <NUM> - second rotary pipe; <NUM> - second discharge channel; <NUM> - second discharge hole; <NUM> - circulating pump; <NUM> - cooler; <NUM> - filter; <NUM> - dryer; <NUM> - discharge pump.

Hereunder some embodiments of the present invention will be detailed with reference to the accompanying drawings. It should be understood that the embodiments described herein are only provided to describe and explain the present invention rather than constitute any limitation to the present invention.

In the present disclosure, unless otherwise specified, the terms that denote the orientations are used as follows, for example: "top", "bottom", "left" and "right" usually refer to "top", "bottom", "left" and "right" as shown in the accompanying drawings; "inside" and "outside" refer to inside and outside in relation to the profiles of the components. Hereunder the present invention will be detailed in embodiments with reference to the accompanying drawings.

In an aspect, the present invention provides an insoluble sulfur production system, which comprises a polymeric kettle <NUM> having a first discharge port and a quenching tower <NUM> having a feed port, wherein the first discharge port is in communication with the feed port, and the quenching tower <NUM> comprises a cylindrical housing <NUM>, a granulation device <NUM> and a shear pump <NUM>, the housing <NUM> comprises a feed quenching section <NUM> and a discharging section <NUM> that are arranged from top to bottom, and the side wall of the housing <NUM> is provided with a solvent inlet <NUM> for providing a solvent and a quenching agent inlet <NUM> for providing a quenchant respectively, wherein:.

The insoluble sulfur production system provided by the present invention can accomplish granulation, quenching, curing extraction, and crushing extraction in the quenching tower and output a slurry material. By granulation in the granulation device <NUM> after the feeding, it can ensure that the material is in a granular state in the follow-up quenching, curing and extraction process, so that the material contacts with the solvent and the quenchant extensively and can form a circulating flow along with the liquid; the shear pump <NUM> and the filter screen <NUM> ensure that the slurry material can be outputted from the second discharge port, thus avoiding clogging in the inner circulating cylinder and the transportation pipeline during subsequent transportation.

Specifically, as shown in <FIG> and <FIG>:
Liquid sulfur is preheated to <NUM>-<NUM> and fed into the polymeric kettle <NUM>; at the same time, an initiator is added into the polymeric kettle <NUM> in an amount equal to <NUM>%-<NUM>% of the amount of the liquid sulfur. The material is heated to <NUM>-<NUM> under nitrogen shielding for polymerization reaction, and is kept at the temperature for <NUM>-<NUM> minutes.

After the polymerization, the liquid sulfur is fed into the quenching tower <NUM> through the feed port; the material is granulated in the granulation device <NUM> first, and then the granular material (i.e., the hot sulfur granules that are formed from liquid drops and have a solid outer layer and a liquid inner core as described below) contacts with the quenchant in the quenching tower <NUM> (the quenchant is introduced into the quenching tower <NUM> through a quenching agent inlet <NUM>, and soft water may be used as the quenchant); the hot sulfur granules are quenched and solidified in the feed quenching section <NUM> and for example , immersed in the quenchant in the inner circulating cylinder <NUM>; the quenching temperature is <NUM>-<NUM>; after quenching for <NUM>-<NUM> minutes, the quenchant is discharged from the quenching tower <NUM> through the second discharge port, and the solid granules formed after quenching are retained in the quenching tower <NUM> by the filter screen <NUM>.

Then, a solvent is fed into the quenching tower <NUM> continuously through the quenching agent inlet <NUM> so as to extract the soluble sulfur continuously; after curing at <NUM>-<NUM> temperature for <NUM>-<NUM> hours, the shear pump <NUM> is started to shear the sulfur granules cyclically at <NUM>-<NUM> for <NUM>-<NUM> minutes; when the sulfur granules are in size smaller than <NUM>, the fine sulfur granules are discharged from the second discharge port through the filter screen <NUM>.

As described above, in the insoluble sulfur production system provided by the present invention, quenching, curing extraction and crushing extraction can be completed without transporting the materials, and finally a slurry material containing fine granules is discharged from the second discharge port, thus the possibility of clogging in the output pipeline is greatly decreased. In addition, by means of continuous quenching, curing extraction and crushing extraction in the quenching tower <NUM>, the processing time can be greatly shortened, the processing equipment and process can be simplified, and the production efficiency can be improved.

In the present invention, during quenching, curing extraction and crushing extraction, the quenchant and solvent can be continuously inputted, while the second discharge port is kept open, so as to maintain the required processing temperature.

Alternatively, in order to reduce the cost and improve the efficiency, the quenchant and solvent may be recycled and reused. Preferably, the insoluble sulfur production system may comprise a cooler <NUM>, and the housing <NUM> comprises a material separation section <NUM> for solid-liquid separation and a material circulation section <NUM> for circulating the materials between the feed quenching section <NUM> and the discharging section <NUM>, an inner circulating cylinder <NUM> and a liquid distributor <NUM> for spraying a quenchant or solvent into the inner circulating cylinder <NUM> are arranged in the material circulating section <NUM>, and a circulating liquid outlet <NUM> for discharging the separated liquid is arranged in the side wall of the material separating section <NUM>, the liquid discharged from the circulating liquid outlet <NUM> is cooled by the cooler <NUM> and sent by the circulating pump <NUM> to the circulating inlet, which is in communication with the liquid distributor <NUM>.

During the quenching, the quenchant in the quenching tower <NUM> flows through the cooler <NUM> from the circulating liquid outlet <NUM> for cooling, is pressurized by the circulating pump <NUM> and circulated into the circulating inlet and sprayed by the liquid distributor <NUM> into the inner circulating cylinder <NUM>, thereby the quenchant is recycled and reused. Likewise, during curing extraction, the solvent flows through the cooler <NUM> from the circulating liquid outlet <NUM> for cooling, is pressurized by the circulating pump <NUM> and circulated into the circulating inlet and sprayed by the liquid distributor <NUM> into the inner circulating cylinder <NUM>, thereby the solvent is recycled and reused; during crushing extraction, the solvent flows through the cooler <NUM> from the circulating liquid outlet <NUM> for cooling, is sheared by the shear pump <NUM> and circulated into the circulating inlet and sprayed by the liquid distributor <NUM> into the inner circulating cylinder <NUM>, thereby the solvent is recycled and reused.

Under the action of cyclic transportation by the circulating pump <NUM> or shear pump <NUM>, the granular material in the inner circulating cylinder <NUM> collides and contacts with the quenchant or solvent extensively and is formed in a fluidized state, thereby the quenching, curing and extraction can be carried out better and more quickly.

The material separation section <NUM> is used to separate the granular material carried in the fluid from the liquid (e.g., the quenchant or solvent), so that the liquid discharged from the circulating liquid outlet <NUM> can be circulated. When the fluid gushes from the upper end of the inner circulating cylinder <NUM> via the circulating pump <NUM>, the flow rate of the fluid is decreased owing to the that the flow section is changed from the cross section of the inner circulating cylinder <NUM> to the cross section of the housing <NUM> suddenly, thus the granular material settles down under gravity action and is separated from the liquid, and the separated granular material is retained in the inner circulating cylinder <NUM> or falls down along the outer wall of the inner circulating cylinder <NUM>. To guide the falling of the granular material, a conical cylinder-shaped circulating flow guide plate <NUM> expanding downward gradually is arranged on the periphery at the top of the inner circulating cylinder <NUM>, and clearance exists between the circulating flow guide plate <NUM> and the inner wall of the housing <NUM>. Preferably, the radius of the lower end of the circulating flow guide plate <NUM> is <NUM>-<NUM> times of the radius of the housing <NUM>, so as to maintain appropriate clearance. The lower end of the circulating flow guide plate <NUM> is located below the circulating liquid outlet <NUM>, so as to prevent the granular material from entering the circulating liquid outlet <NUM> when the quenchant or solvent is circulated.

In addition, preferably, a conical cylinder-shaped material flow guide plate <NUM> tapered toward the inner circulating cylinder <NUM> may be arranged on the inner wall of the material separation section <NUM>. Thus, the granular material formed through granulation can be guided by the material flow guide plate <NUM> into the inner circulating cylinder <NUM>. To avoid interference with solid-liquid separation, the material flow guide plate <NUM> is located above the circulating liquid outlet <NUM>.

Preferably, in order to guide the material into the inner circulating cylinder <NUM> at an appropriate speed under the guidance of the material flow guide plate <NUM>, the material flow guide plate <NUM> is arranged in at least one of the following forms:.

In addition, the corresponding components and parameters of the material circulation section <NUM> and the discharging section <NUM> may be set to retain the material in the material circulation section <NUM> and the discharging section <NUM> for a required duration; preferably, the insoluble sulfur production system is configured in at least one of the following forms:.

In the present invention, the solvent inlet <NUM> and the quenching agent inlet <NUM> may be arranged at appropriate positions of the housing <NUM>, and may be connected to corresponding external storage devices through corresponding pipelines. Preferably, the solvent inlet <NUM> and the quenching agent inlet <NUM> may be arranged in the side wall of the feed quenching section <NUM>, so as to avoid interference with the operation of other sections (e.g., the material separation section <NUM>).

In the present invention, the granulation device <NUM> may be in any appropriate form, as long as the material entrying from the feed port can be formed into granular material. The material fed from the feed port is usually in a liquid state in which the material is drawn and difficult to granulate; the granulation device <NUM> may be arranged to separate and granulate the material into a droplet-shaped granular material (also referred to as droplet material).

According to a preferred embodiment of the present invention, as shown in <FIG>, the granulation device <NUM> comprises a first feed pipe <NUM> in communication with the feed port and a first distribution pipe <NUM> in communication with the first feed pipe <NUM>, the first distribution pipe <NUM> comprises a first fixed pipe <NUM> and a first rotary pipe <NUM> that is sleeved on the first fixed pipe <NUM> and can rotate with respect to the first fixed pipe <NUM>, the pipe wall of the first fixed pipe <NUM> is provided with a first discharge channel <NUM> extending in the axial direction, the pipe wall of the first rotary pipe <NUM> is provided with multiple groups of first discharge holes <NUM> that can correspond to the first discharge channel <NUM>, each group of first discharge holes <NUM> are arranged in the axial direction, and the multiple groups of first discharge holes <NUM> are distributed in the circumferential direction of the first rotary pipe <NUM>.

In use, the material fed from the feed port flows through the first feed pipe <NUM> into the first fixed pipe <NUM>, and is rotated upward through the first rotary pipe <NUM> to the first discharge holes <NUM> aligned to the first discharge channel <NUM> and then discharged. The first rotary pipe <NUM> is rotated with respect to the first fixed pipe <NUM>, so as to discharge the material intermittently through different first discharge holes <NUM>; thus the material can be cut by means of the counter-rotation to form a droplet material corresponding to the shape of the first discharge holes <NUM> and realize granulation. In order to obtain a droplet material in an appropriate size, the shape and parameters of the first discharge holes <NUM> may be arranged appropriately; preferably, the first discharge holes <NUM> may be in size of <NUM>-<NUM>, and the spacing between adjacent first discharge holes <NUM> in the same group may be <NUM>-<NUM>. The size of the first discharge holes <NUM> refers to the maximum dimension of the shape contour, and may vary depending on the shape of the first discharge holes <NUM>. For example, in the case of circular first discharge holes <NUM>, the size is the diameter; for elliptical first discharge holes <NUM>, the size is the major diameter of the ellipse; for rectangular first discharge holes <NUM>, the size is the length of the longer side.

In addition, in order to enable the quenchant to contact with the material extensively in the feed quenching section <NUM>, a distributor for uniformly distributing the quenchant may be arranged in the feed quenching section <NUM>. In a preferred embodiment of the present invention, as shown in <FIG>, the feed quenching section <NUM> is provided with a quenchant distributor <NUM>, which comprises a second feed pipe <NUM> in communication with the quenching agent inlet <NUM> and a second distribution pipe <NUM> in communication with the second feed pipe <NUM>, wherein the second distribution pipe <NUM> is arranged in parallel to the first distribution pipe <NUM> , the setting height of the second distribution pipe <NUM> is lower than the first distribution pipe <NUM>, and the second distribution pipe <NUM> comprises a second fixed pipe <NUM> and a second rotary pipe <NUM> that is sleeved on the second fixed pipe <NUM> and can rotate with respect to the second fixed pipe <NUM>, the pipe wall of the second fixed pipe <NUM> is provided with a second discharge channel <NUM> extending in the axial direction, the pipe wall of the second rotary pipe <NUM> is provided with multiple second discharge holes <NUM> that can correspond to the second discharge channel <NUM> and are distributed in the circumferential direction of the second rotary pipe <NUM>, the outer wall of the second rotary pipe <NUM> is provided with a doctor blade <NUM> that can come into contact with the outer wall of the first rotary pipe <NUM>, the first discharge channel <NUM> is arranged toward the second distribution pipe <NUM>, and the second discharge channel <NUM> is arranged offset from the first distribution pipe <NUM>.

In use, the quenchant flows through the second feed pipe <NUM> into the second fixed pipe <NUM>, and is rotated upward by the second rotary pipe <NUM> to the second discharge holes <NUM> aligned to the second discharge channel <NUM> and then discharged.

Since the quenchant is supplied to the quenching agent inlet <NUM> at certain pressure, it will be discharged from the second discharge holes <NUM> in the form of jetting. In order to provide the quenchant uniformly along the second distribution pipe <NUM>, each second discharge hole <NUM> comprises a plurality of slits extending in the axial direction sequentially, and each slit is in <NUM>-<NUM> width; and/or the second discharge holes <NUM> are configured to provide the quenchant in the tangential direction of the second rotary pipe <NUM>.

By arranging the second discharge channel <NUM> offset from the first distribution pipe <NUM> (i.e., the second discharge channel <NUM> is not between the first rotary pipe <NUM> and the second rotary pipe <NUM>), the jetted quenchant will not contact immediately with the droplet material discharged from the first discharge holes <NUM> and cause clogging of the first discharge holes <NUM> by the droplets chilled suddenly. By orienting the first discharge channel <NUM> toward the second distribution pipe <NUM> (i.e., the first discharge channel <NUM> is located between the first rotary pipe <NUM> and the second rotary pipe <NUM>, preferably the first discharge channel <NUM> is located in a connecting line between the centers of circles of the first rotary pipe <NUM> and the second rotary pipe <NUM> on the same cross section), when the second rotary pipe <NUM> is rotated, it can come into contact with the outer wall of the first rotary pipe <NUM> through the doctor blade <NUM> , thereby on one hand the drawn material can be cut into a droplet shape thoroughly to facilitate granulation, and on the other hand the material on the outer ends of the first discharge holes <NUM> can be scraped off, so as to prevent the drawn material from adhering to the first discharge holes <NUM> and prevent clogging of the first discharge holes <NUM> incurred by the chilling of the material exposed to a low-temperature environment, thereby solve the problem that it is difficult to granulate the high-viscosity drawn material. More specifically, as shown in <FIG>, the first discharge channel <NUM> is open obliquely downward toward the second distribution pipe <NUM>, and the second discharge channel <NUM> is open obliquely downward toward the side where the first distribution pipe <NUM> is located.

The doctor blade <NUM> is preferably arranged to pass by the outer ends of the first discharge holes <NUM> in a tangential manner. To attain that effect and avoid hard collision between the doctor blade <NUM> and the first rotary pipe <NUM> during the relative movement of the doctor blade <NUM> and the first rotary pipe <NUM>, the doctor blade <NUM> is an elastic doctor blade. In that case, the doctor blade <NUM> may be dimensioned so that it extends beyond the minimum clearance between the first rotary pipe <NUM> and the second rotary pipe <NUM>, thereby the doctor blade <NUM> is deformed elastically to have a portion essentially in the tangential direction of the first rotary pipe <NUM> when the doctor blade <NUM> comes into contact with the first rotary pipe <NUM>, thereby the material is scraped off by that portion. In addition, the doctor blade may be made of a material to which the sulfur material can't adhere easily, in order to avoid adherence of the sulfur material to the doctor blade. Preferably, the doctor blade <NUM> is a stainless steel blade to make the requirements for elasticity and non-adherence.

In the present invention, the cooling of the droplet material discharged from the first discharge holes <NUM> starts from the moment the droplet material leaves the first discharge holes <NUM> to form into hot sulfur granules that have a solid outer layer and a liquid inner core; then the droplets contact with the quenchant extensively in the falling process in the quenching tower, and finally fall into the inner circulating cylinder <NUM> and are immersed in the quenchant and cooled into solid granules.

Preferably, in order to distribute the granular material and the quenchant uniformly, as shown in <FIG>, the first distribution pipe <NUM> and the second distribution pipe <NUM> are a plurality of distribution pipes that are arranged corresponding to each other alternatively, the plurality of first distribution pipes <NUM> are arranged side by side, the plurality of second distribution pipes <NUM> are arranged side by side, and a connecting line between the centers of cross sections of a first distribution pipe <NUM> and a corresponding second distribution pipe <NUM> in the same plane is at <NUM>-<NUM>° with respect to the plane of arrangement of the first distribution pipes <NUM>. The first distribution pipe <NUM> and the second distribution pipe <NUM> may be rake-formed distribution pipes and arranged in the transverse direction of the feed quenching section <NUM>, so as to distribute the material and the quenchant uniformly on the entire cross section of the feed quenching section <NUM>.

By arranging the first distribution pipe <NUM> and the second distribution pipe <NUM> in parallel to each other, the rotation axis of the first rotary pipe <NUM> is parallel to that of the second rotary pipe <NUM>, so that the first rotary pipe <NUM> and the second rotary pipe <NUM> can be rotated by the same driving device. Specifically, the first rotary pipe <NUM> and the second rotary pipe <NUM> may be connected to the driving device via a transmission device respectively. In addition, the first rotary pipe <NUM> and the second rotary pipe <NUM> preferably rotate in the same direction, so as to improve the scraping effect of the doctor blade <NUM>.

In addition, as shown in <FIG>, the insoluble sulfur production system may comprise a washing filter <NUM> and a dryer <NUM>, and the inlet and outlet of the washing filter <NUM> are in communication with the second discharge port and the dryer <NUM> respectively. Specifically, the washing filter <NUM> and the second discharge port may be connected through a pipeline between them, and transportation pressure may be provided in the pipeline by means of the discharge pump <NUM>. The slurry material discharged from the discharge port may be conveniently sent to the washing filter <NUM> by the discharge pump <NUM> for further washing, extraction and filtration treatment, and the washing and filtering solvent may be recycled through a separate pipeline. The washing and filtration temperature is <NUM>-<NUM>, and the washing and filtration operation is carried out continuously for <NUM>-<NUM> times. The insoluble sulfur obtained through filtration enters the dryer <NUM>, for vacuum drying at <NUM>-<NUM> drying temperature for <NUM>-<NUM> hours at <NUM>-<NUM>,000Pa drying vacuum degree, thus an insoluble sulfur product is obtained after the drying.

In a preferred embodiment of the present application, the granulation device <NUM>, circulating pump <NUM>, shear pump <NUM>, inner circulating cylinder <NUM> and liquid distributor <NUM> etc. can realize uniform distribution of the temperature field during material quenching, as well as integrated operation of curing extraction and crushing extraction.

After material feeding, the insoluble sulfur production method provided by the present invention can accomplish granulation, quenching, curing extraction, and crushing extraction sequentially in the quenching tower and output a slurry material. By granulation after the feeding, it can ensure that the material is in a granular state in the follow-up quenching, curing and extraction process, so that the material contacts with the solvent and the quenchant extensively and can form a circulating flow along with the liquid; a slurry material can be obtained by liquid-phase circulated crushing, so as to avoid clogging in the transportation pipeline during subsequent transportation; the granulation device, circulating pump, shear pump, inner circulating cylinder and liquid distributor etc. can realize uniform distribution of the temperature field during material quenching, as well as integrated operation of curing extraction and crushing extraction.

The liquid-phase circulated crushing may be carried out in an appropriate way, for example, by using a shear pump. The slurry material may be filtered when it is outputted.

Preferably, the method comprises: S5. outputting the slurry obtained through liquid-phase circulated crushing from the quenching tower for washing filtration; S6. drying the solid product obtained through washing filtration to obtain an insoluble sulfur product. The slurry material discharged from the quenching tower may be conveniently sent to, for example, the washing filter <NUM> for further washing, extraction and filtration treatment, and the washing and filtering solvent may be recycled through a separate pipeline. The washing and filtration temperature is <NUM>-<NUM>, and the washing and filtration operation is carried out continuously for <NUM>-<NUM> times. The insoluble sulfur obtained through filtration enters, for example, a dryer <NUM>, for vacuum drying at <NUM>-<NUM> drying temperature for <NUM>-<NUM> hours at <NUM>-<NUM>,000Pa drying vacuum degree, thus an insoluble sulfur product is obtained after the drying.

In the insoluble sulfur production method in the present invention, the polymerization temperature may be <NUM>-<NUM>, preferably <NUM>-<NUM>; and the polymerization duration may be <NUM>-<NUM> minutes, preferably <NUM>-<NUM> minutes.

In the insoluble sulfur production method in the present invention, the initiator may be one or more of potassium persulfate, dimethyl sulfoxide, etc. The feed amount of the initiator is <NUM>. 05wt%-<NUM>. 3wt%, preferably <NUM>. 1wt%-<NUM>. 2wt% of the feed amount of the liquid sulfur.

In the insoluble sulfur production method in the present invention, the quenching temperature may be <NUM>-<NUM>, preferably <NUM>-<NUM>; and the quenching duration may be <NUM>-<NUM> minutes, preferably <NUM>-<NUM> minutes.

In the insoluble sulfur production method in the present invention, the quenchant may be soft water.

In the insoluble sulfur production method in the present invention, the solvent used in the curing, washing and filtering process may be one or more of cyclohexane, benzene, paraxylene, etc., preferably is paraxylene.

In the insoluble sulfur production method in the present invention, the curing temperature may be <NUM>-<NUM>, preferably <NUM>-<NUM>; the curing duration may be <NUM>-<NUM> hours, preferably <NUM>-<NUM> hours. The extraction agent is used as the curing solvent, so as to carry out sulfur granule curing and extraction at the same time; thus, compared with the conventional low-temperature melting method, the curing time is shortened, a quenchant drying process can be avoided, the technical process is greatly shortened, the process flow is simplified, and the production efficiency is improved.

In the insoluble sulfur production method provided by the present invention, the processing temperature of the liquid-phase circulated crushing may be <NUM>-<NUM>, preferably <NUM>-<NUM>, the processing time may be <NUM>-<NUM> minutes, preferably <NUM>-<NUM> minutes, and the granularity of the granules after the crushing may be <NUM>-250mpi, preferably <NUM>-200mpi. The extraction agent is used as the solvent for the liquid-phase circulated crushing, and sulfur granule crushing and extraction are carried out at the same time; compared with the conventional dry mechanical crushing method, the adverse effect of increased material temperature on the product quality during the crushing can be avoided.

In the insoluble sulfur production method provided by the present invention, the temperature of washing filtration may be <NUM>-<NUM>, preferably <NUM>-<NUM>, and the washing filtration is carried out continuously for <NUM>-<NUM> times, preferably <NUM>-<NUM> times.

In the insoluble sulfur production method provided by the present invention, the drying may be vacuum drying, the drying temperature may be <NUM>-<NUM>, preferably <NUM>-<NUM>, the drying duration may be <NUM>-<NUM> hours, preferably <NUM>-<NUM> minutes, and the vacuum degree of drying may be <NUM>-<NUM>,000Pa, preferably <NUM>-500Pa.

Claim 1:
An insoluble sulfur production system, comprising a polymeric kettle (<NUM>) having a first discharge port and a quenching tower (<NUM>) having a feed port, wherein the first discharge port is in communication with the feed port, and the quenching tower (<NUM>) comprises a cylindrical housing (<NUM>), a granulation device (<NUM>) and a shear pump(<NUM>), the housing (<NUM>) comprises a feed quenching section (<NUM>) and a discharging section (<NUM>) that are arranged from top to bottom, and the side wall of the housing (<NUM>) is provided with a solvent inlet (<NUM>) for providing a solvent and a quenching agent inlet (<NUM>) for providing a quenchant, wherein:
the feed port is arranged on the feed quenching section (<NUM>), and the granulation device (<NUM>) is arranged near the feed port and positioned in the feed quenching section (<NUM>);
the discharging section (<NUM>) is provided with a second discharge port and a filter screen (<NUM>) above the second discharge port, and the side wall of the discharging section (<NUM>) is provided with a circulating outlet and a circulating inlet in communication with an inlet and an outlet of the shear pump (<NUM>) respectively above the filter screen (<NUM>).