CN114100473A - Continuous oil filling method and oil filling mixing device for insoluble sulfur - Google Patents
Continuous oil filling method and oil filling mixing device for insoluble sulfur Download PDFInfo
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Abstract
The invention discloses a continuous oil-filling method and an oil-filling mixing device for insoluble sulfur, wherein the method comprises the following steps: the insoluble sulfur dry powder continuously falls onto a material distribution disc rotating in an oil-filled mixing device through a material inlet pipe, and the insoluble sulfur dry powder continuously falls into the bottom of the device along the edge of the material distribution disc; continuously spraying mineral oil in a spraying mode while adding the insoluble sulfur dry powder, so that the insoluble sulfur and the mineral oil are sprayed and fully mixed in the falling process; and discharging the insoluble sulfur and the mineral oil which are uniformly mixed at the bottom of the device from a discharge hole. The insoluble sulfur is dispersed in the mixing device in a material distribution disc mode, the mineral oil is contacted with the insoluble sulfur in an atomization mode, the oil filling process is completed instantly, and the production efficiency is obviously improved. The oil filling process is completed instantly, the mineral oil and the insoluble sulfur are contacted and mixed evenly, the oil filling time is greatly shortened, the influence on the content and the thermal stability of the insoluble sulfur is reduced to the maximum extent, and the product quality is improved.
Description
Technical Field
The invention relates to a continuous oil-filling method for insoluble sulfur and an oil-filling mixing device used by the method, belonging to the technical field of insoluble sulfur preparation.
Background
Insoluble sulfur is a rubber vulcanizing agent having excellent properties, and can be classified into an oil-extended type and a non-oil-extended type depending on whether oil is extended during the post-treatment. Because the non-oil-filled insoluble sulfur has the defects of small particle size, easy flying, large using dust, difficult dispersion in mixing, flammability, explosiveness and the like, the oil-filled insoluble sulfur is commonly used in the rubber processing and tire industry.
At present, the preparation of oil-filled insoluble sulfur mainly adopts an intermittent production process, which is simply described as follows: and (3) putting the insoluble sulfur dry powder and the mineral oil into a mixer at one time according to a certain proportion, stirring for a certain time, detecting whether the oil content is qualified, discharging and packaging. Due to large feeding amount and long mixing time, the heat stability and the content of insoluble sulfur are reduced, and the method is one of important factors influencing the product quality. Therefore, insoluble sulfur manufacturers continuously explore and innovate and search for a new oil filling mode.
For example, chinese patent CN 204134500U discloses an oil filling device for insoluble sulfur, which uses a screw propeller to fill oil. The spiral propeller pipe wall is provided with a plurality of oil filling ports, insoluble sulfur is pushed by the spiral blades to move along the axial direction of the rotating shaft and is stirred by the spiral blades, and the insoluble sulfur moves and is sequentially contacted and mixed with oil entering through the oil filling ports, so that the purpose of continuous oil filling is achieved. However, the helical blade has an axial pushing effect and small shearing force, and the uniform mixing of insoluble sulfur and oil products cannot be ensured.
Chinese patent CN 10820381A discloses a production method and production equipment of oil-filled insoluble sulfur, which heats powdered insoluble sulfur which is not completely desolventized and mineral oil together in the desolventizing step, so that carbon disulfide which is remained in the powdered insoluble sulfur which is not completely desolventized is dissolved in the mineral oil and escapes, and the effect of complete desolventizing is achieved. Because carbon disulfide has certain solubility in mineral oil, the desolventizing time is relatively long, and certain influence is caused on the physicochemical indexes of insoluble sulfur.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a continuous oil-filling method for insoluble sulfur, which continuously feeds insoluble sulfur dry powder into a mixing device, and mineral oil is mixed in a spraying manner, so that the two are instantly and uniformly mixed, the oil filling is instantly completed, the operation time is obviously shortened, the production efficiency of the oil filling process is improved, the influence of the mixing process on the thermal stability and content of the insoluble sulfur is reduced to the greatest extent, and the effect of improving the product quality is achieved.
The technical scheme of the invention is as follows:
a continuous oil-filling method of insoluble sulfur comprises the following steps:
(1) the insoluble sulfur dry powder continuously falls onto a material distribution disc rotating in an oil-filled mixing device through a dry powder feeding pipe, and the insoluble sulfur dry powder continuously falls into the bottom of the oil-filled mixing device along the edge of the material distribution disc under the drive of the material distribution disc;
(2) continuously spraying mineral oil into an oil-filled mixing device in a spraying mode while adding the insoluble sulfur dry powder, so that the insoluble sulfur dry powder is fully mixed with mineral oil spray in the falling process;
(3) and discharging the insoluble sulfur and the mineral oil which are uniformly mixed at the bottom of the oil-filled mixing device from a discharge hole.
In the method, the insoluble sulfur dry powder and the mineral oil are respectively and accurately conveyed to the oil-filled mixing device by a continuous conveying device with a metering and adjusting function according to a proportion, and feeding and metering equipment of the insoluble sulfur dry powder can be a weightless feeding scale, a powder material quantitative feeding machine, a solid material flow meter (including a chute type and an impulse type), a rotor scale (including a Fisher type and a powder grinding type), a Coriolis mass flow meter, a screw scale, a powder material nucleon scale and the like, preferably the weightless feeding scale.
Furthermore, the feeding speed of the insoluble sulfur dry powder is 140-160kg/min, and the mass ratio of the feeding amount of the insoluble sulfur to the feeding amount of the mineral oil in unit time is about 8: 2. Within this range, the insoluble sulfur dry powder is better mixed with the atomized mineral oil during the falling process.
Further, the mineral oil is white oil or naphthenic oil.
Further, the small droplets in the mineral oil spray have a particle size in the range of 1 to 100. mu.m, preferably 30 to 50 μm. The atomization of the mineral oil can be achieved by means of atomization which is customary today, for example by means of an atomizer, for example by means of a pressure device, for example a pressure pump, gas pressure, etc.
Furthermore, the rotating speed of the cloth disc is 20-100r/min, preferably 40 r/min. Insoluble sulfur dry powder falls into cloth dish on the back, can make insoluble sulfur dry powder evenly distributed on the cloth dish through the rotation, and along with the increase of insoluble sulfur dry powder, it can evenly fall along the edge of cloth dish, at the in-process that falls, insoluble sulfur dry powder is cylindrically, a columniform material curtain has been formed, mineral oil distributes in the oil filling mixing arrangement with the form of droplet, the even surface of spraying at the material curtain in the in-process of insoluble sulfur whereabouts, mineral oil and insoluble sulfur's even mixture in the twinkling of an eye has been realized. In addition, the contact surface of the mineral oil and the insoluble sulfur in unit area is large and sufficient, the amount is small, the local overheating phenomenon is reduced, the content of the insoluble sulfur is improved, and the product quality is ensured.
Further, the diameter control ratio of the material distribution disc to the oil-filled mixing device is 2:10-6:10, preferably 4: 10. such diameter setting is matched with the rotating speed, the feeding speed of materials and the mineral oil particle size, and has a better effect.
Furthermore, the invention also provides a preferable mode, the bottom of the oil-filled mixing device is also provided with a high-speed shearing structure, the material falling on the high-speed shearing structure can be scattered, the mixing is more uniform, the shearing speed is 400-. The mixing effect is further improved by the addition of the stirring step.
Furthermore, the invention also provides a preferable mode, a cold air circulating system is also arranged in the oil-filled mixing device, and the cold air circulating system is started from the beginning of adding the insoluble sulfur dry powder, so that flowing gas always exists in the whole oil-filled mixing device, the flowing direction of the gas flows from the bottom of the kettle body to the top of the kettle body, the wind pressure of the circulating cold air is 0.01MPa-0.1MPa, preferably 0.04MPa, the temperature of each part of the oil-filled mixing device can be kept to be 20 ℃ -35 ℃ (preferably 20 ℃ -25 ℃), the insoluble sulfur dry powder can be ensured to be in a suspension state, and the insoluble sulfur dry powder can be more conveniently mixed with mineral oil. Compare with insulation construction such as heat preservation jacket, the cold wind circulation system can be better realize fill the invariant of temperature among the oil mixing arrangement, improve heat exchange efficiency, the better quality that promotes the insoluble sulfur. The cold air circulating system can be used together with the high-speed shearing structure, and can also be used independently.
Furthermore, the whole oil-filled mixing process is carried out in a nitrogen environment, and the existence of nitrogen can improve the safety of the whole process. For example, mineral oil spray uses nitrogen as a carrier, and nitrogen is circulated in an oil-filled mixing device in a cold air circulation system.
Further, the cold air circulation system maintains the pressure of the circulating nitrogen gas in the oil-filling mixing device at 0.01MPa to 0.1MPa, preferably 0.04 MPa. Under the pressure, the insoluble sulfur can be ensured to be in a suspension state in the oil-filled mixing device, and the mixing is more uniform.
Furthermore, the insoluble sulfur and the mineral oil which are fully and uniformly mixed are continuously or intermittently discharged from a discharge hole at the bottom of the oil-filled mixing device, the oil-filled mixing device is ensured not to be emptied during discharging, and a mixture of partial insoluble sulfur and mineral oil exists in the kettle all the time.
The invention also provides an oil-charging mixing device required by the continuous oil charging of the insoluble sulfur, which comprises a kettle body, wherein the kettle body is provided with a hollow cavity, a material distribution structure is also arranged in the kettle body, the material distribution structure is positioned at the upper part of the kettle body and comprises a motor positioned at the top of the kettle body, the output end of the motor is connected with a stirring rod, the tail end of the stirring rod is connected with a horizontally arranged material distribution plate, the upper part of the kettle body is provided with a dry powder feeding pipe, and the outlet of the dry powder feeding pipe is positioned above the material distribution plate, so that the insoluble sulfur dry powder is ensured to fall onto the material distribution plate; still be equipped with a plurality of mineral oil inlet pipes on the cauldron body lateral wall, the export of every mineral oil inlet pipe all is connected with atomizer, atomizer is located the below of cloth dish, and atomizer uses cloth dish to enclose into the diameter of a circle that circular and atomizer formed as the axle center and is greater than cloth dish diameter, and each atomizer's material blowout direction is perpendicular with the decline direction of insoluble sulphur.
Furthermore, the cloth dish is a circular flat board, evenly is provided with the micropore on it, is the fretwork form, prevents that insoluble sulphur from adhering to cloth dish upper surface. The micropores ensure that the insoluble sulfur cannot fall off.
Preferably, the outlet of the dry powder feeding pipe is positioned right above the material distribution plate, or a splitter plate can be further arranged on the material distribution plate, so that the uniform distribution of the insoluble sulfur dry powder on the material distribution plate is better ensured.
Further, the diameter control ratio of the material distribution disc to the oil-filled mixing device is 2:10-6:10, preferably 4: 10.
furthermore, the number of the atomizing nozzles is more than or equal to 2, preferably 4, that is, the number of the mineral oil feeding pipes is more than or equal to 2, and the number of the atomizing nozzles is selected to ensure that all falling insoluble sulfur can be fully contacted and mixed with the spray, preferably 4. Each atomizer is located same horizontal plane, forms a circular, is located the below of cloth dish, and the interval between the atomizer is the same.
Further, the mineral oil may be atomized by installing a pressurizing device, such as a pressurizing pump, a gas pressurizing device, or the like, preferably a nitrogen pressurizing device, on the mineral oil feed pipe in front of the atomizing nozzle.
Further, the lower part in the kettle body is provided with a high-speed shearing structure, the high-speed shearing structure is positioned at the lower part of the kettle body, the materials falling on the high-speed shearing structure are sheared and scattered below the atomizing spray head, and the high-speed shearing structure comprises at least one stirrer. The stirrers are arranged on the side wall of the kettle body, and the stirrers are preferably uniformly distributed. The number of the stirrers ensures that the stirrers can sufficiently shear the materials falling from the upper part, and 3 stirrers are preferred.
Further, the stirrer may be a paddle stirrer, a propeller stirrer, an anchor stirrer, or the like, preferably a paddle stirrer, such as a paddle stirrer.
Furthermore, a heat-insulating jacket or a cold air circulating system is also arranged on the kettle body and used for maintaining the temperature of the kettle body. The cold air circulating system comprises an air inlet pipe and an air outlet pipe, the air inlet pipe enters the lower part of the kettle body through an air inlet in the kettle body, one end of the air inlet pipe is positioned in the kettle body, the other end of the air inlet pipe is connected with a fan, one end of the air outlet pipe is connected with an air outlet in the top of the kettle body, the other end of the air outlet pipe is connected with the fan, a condenser is arranged between the air inlet pipe and the fan, and nitrogen coming out of the fan is cooled to the required temperature and then discharged into the kettle body. Gas enters from the bottom of the kettle body, and is discharged from the top, and the dispersion and suspension of insoluble sulfur are enhanced by the flowing direction and certain pressure of circulating gas.
Further, the bottom of the kettle body is provided with a discharge port, the discharge port is connected with a continuous conveying device in a sealing mode, and the continuous conveying device is preferably a double-shaft screw conveyor. And the continuous conveying device continuously conveys the mixed oil powder to downstream packaging equipment so as to finish the oil filling process.
The invention has the following beneficial effects:
1. the insoluble sulfur is dispersed in the mixing device in a material distribution disc mode, the mineral oil is contacted with the insoluble sulfur in an atomization mode, the oil filling process is completed instantly, and the production efficiency is obviously improved.
2. The oil filling process is completed instantly, the mineral oil and the insoluble sulfur are contacted and mixed evenly, the oil filling time is greatly shortened, the influence on the content and the thermal stability of the insoluble sulfur is reduced to the maximum extent, and the product quality is improved.
3. The invention improves the mixing device, adds the material distribution disc, the atomizing spray head and the cold air circulating system, greatly improves the contact efficiency and the heat transfer efficiency of the insoluble sulfur and the mineral oil, and improves the production efficiency and the quality of the insoluble sulfur.
Drawings
FIG. 1 is a schematic structural diagram of an oil-filled mixing device for insoluble sulfur according to the present invention.
In the figure, 1, a dry powder feeding pipe; 2. a material distribution disc; 3. a mineral oil feed pipe; 4. a condenser; 5. an atomizing spray head; 6. a high speed shear configuration; 7. a fan; 8. a continuous conveying device.
Detailed Description
The present invention will be described in further detail below with reference to specific examples. However, these specific examples are only for explaining the present invention and are not intended to limit the present invention.
Example 1
As shown in fig. 1, the oil-filled mixing device of insoluble sulfur with a preferred structure of the invention comprises a kettle body, wherein the kettle body is provided with a hollow cavity, a material distribution structure is arranged in the kettle body, the material distribution structure is positioned at the upper part of the kettle body and comprises a motor positioned at the top of the kettle body, the output end of the motor is connected with a stirring rod, the tail end of the stirring rod is connected with a horizontally arranged material distribution disc, the material distribution disc is a circular flat plate, micropores are uniformly arranged on the material distribution disc, and are hollow, and the insoluble sulfur cannot fall off from the micropores. The upper part of the kettle body is provided with a dry powder feeding pipe, and the outlet of the dry powder feeding pipe is positioned above the distributing plate, so that the insoluble sulfur dry powder is ensured to fall onto the distributing plate. Still be equipped with a plurality of mineral oil inlet pipes on the cauldron body lateral wall, the export of every mineral oil inlet pipe all is connected with an atomizer, atomizer is located the below of cloth dish, and each atomizer is located same horizontal plane, and the interval between the atomizer is the same, and atomizer uses the cloth dish to enclose into the diameter of a circle that circular and atomizer formed as the axle center and is greater than cloth dish diameter, and each atomizer's material blowout direction is perpendicular with the decline direction of insoluble sulphur. The number of the atomizing nozzles is selected to ensure that all falling insoluble sulfur can be fully contacted and mixed with the spray by the sprayed mineral oil, and the number of the atomizing nozzles is more than or equal to 2, preferably 4.
And a high-speed shearing structure is also arranged at the lower part in the kettle body, and comprises at least one stirrer, preferably 3 stirrers. The stirrers are arranged on the side wall of the kettle body, and the stirrers are preferably uniformly distributed. The stirrer may be a paddle stirrer, propeller stirrer, anchor stirrer or the like, preferably a paddle stirrer, such as a paddle stirrer.
The kettle body is also provided with a cold air circulating system for maintaining the temperature of the kettle body. The cold air circulating system comprises an air inlet pipe and an air outlet pipe, the air inlet pipe enters the lower part of the kettle body through an air inlet in the kettle body, air discharged from the air inlet pipe flows in the direction from the bottom of the kettle to the top of the kettle, one end of the air inlet pipe is positioned in the kettle body, the other end of the air inlet pipe is connected with a fan, the air outlet pipe is connected with an air outlet in the top of the kettle body, the other end of the air outlet pipe is connected with the fan, a condenser is arranged between the air inlet pipe and the fan, and nitrogen coming out of the fan is cooled to the required temperature and then discharged into the kettle body. Gas enters from the bottom of the kettle body, and is discharged from the top, so that the temperature in the kettle body is maintained, and the dispersion and suspension of insoluble sulfur are enhanced. The cold air circulating system circulates nitrogen.
And a discharge port is arranged at the bottom of the kettle body and is connected with a continuous conveying device in a sealing manner, and the continuous conveying device is preferably a double-shaft screw conveyor. And the continuous conveying device continuously conveys the mixed oil powder to downstream packaging equipment so as to finish the oil filling process.
The process of adopting the oil-filled mixing device to realize continuous oil filling comprises the following steps:
1. the insoluble sulfur dry powder and the mineral oil are continuously conveyed into an oil-filled mixing device according to the proportion;
2. the insoluble sulfur dry powder enters an oil filling and mixing device and falls on a material distribution disc by gravity, and the dry powder forms a stable cylindrical material curtain at the edge of the material distribution disc and falls at a constant speed in the process of constant speed rotation of the material distribution disc;
3. a plurality of atomizing nozzles are arranged around the periphery of the material curtain, and the mineral oil is sprayed out in a small liquid drop mode through the atomizing nozzles and uniformly sprayed on the surface of the material curtain;
4. the high-speed shearing structure and the cold air circulating system below the atomizing spray head ensure that the temperature of the materials does not change obviously while the insoluble sulfur dry powder and the mineral oil are instantly mixed fully and uniformly.
5. Realize the oily powder after abundant homogeneous mixing and be carried to low reaches equipment for packing by continuous conveyor, further stir in the transportation process, not only make oily powder further mix, inside mineral oil entered into the powder by insoluble sulfur powder surface simultaneously, more can guarantee oil content's stability.
Example 2
The structure of the oil-filled mixing device for insoluble sulfur is the same as that of the embodiment 1, except that: does not contain a cold air circulating system, but a heat-insulating jacket is arranged on the outer side of the kettle body, and flowing condensed water or condensed oil is arranged in the heat-insulating jacket and used for keeping the temperature.
Example 3
An oil-filled mixing device with the volume of 8 cubes is selected, the structure of the oil-filled mixing device is the same as that of the oil-filled mixing device in embodiment 1, and the ratio of the diameter of the material distribution disc to the diameter of the kettle body is 4: 10. adding insoluble sulfur dry powder into an oil filling mixing device by a weight loss scale, wherein the feeding speed is 160 kg/min. The powder falls to the surface of the material distribution disc by means of gravity, the material distribution disc is set to rotate at a speed of 40r/min, and the dry powder forms a stable cylindrical material curtain at the edge of the material distribution disc and falls at a constant speed. 4 atomizing nozzles are uniformly arranged around the material curtain, naphthenic oil is sprayed to the surface of the material curtain through each atomizing nozzle, the particle diameter of small droplets of the naphthenic oil is 30-50 mu m, and the total feeding speed of the naphthenic oil is 40 kg/min. 3 paddle type stirrers are uniformly arranged below the atomizing spray head, the rotating speed is controlled to be 800r/min, and the operation of a cold air circulating system is controlled at the same time, so that the air pressure of nitrogen circulation is 0.04MPa, and the temperature is 25 ℃. The oil charge powder that falls to the bottom shifts to low reaches equipment for packing through biax screw conveyer, accomplishes the continuous oil charge process, arranges the material and guarantees not empty cauldron among the oil charging mixing arrangement, oil charge speed: 12 ton/h.
The obtained insoluble sulfur product is detected according to GB/T18952-2017, and has an insoluble sulfur content of 97.8% and a thermal stability (105 ℃ 15 min) of 89.7%. 3 time points of discharging for 5min, 20min and 30min are respectively sampled and detected in the oil-filled mixing device, the oil content in insoluble sulfur detection is respectively 20.0%, 20.0% and 20.0%, and the stability of the oil content index is good.
Example 4
The procedure of example 3 was used to extend the oil, with the following differences: set up the quantity of atomizer to 3, accomplish the continuous oil filling process, oil filling speed: 12 t/h.
The obtained insoluble sulfur product is detected according to GB/T18952-2017, and has an insoluble sulfur content of 97.1% and a thermal stability (105 ℃ 15 min) of 89.2%. 3 time points of discharging for 5min, 20min and 30min are respectively sampled and detected in the oil-filled mixing device, the oil content in insoluble sulfur detection is respectively 20.0%, 21.0% and 19.5%, and the oil content index has small fluctuation.
Example 5
The procedure of example 3 was used to extend the oil, with the following differences: adjusting the paddle type stirring control rotating speed to 400r/min, keeping other control parameters unchanged, completing the continuous oil filling process, wherein the oil filling speed is as follows: 12 t/h.
The obtained insoluble sulfur product is detected according to GB/T18952-2017, and has an insoluble sulfur content of 97.6% and a thermal stability (105 ℃ 15 min) of 89.6%. 3 time points of discharging for 5min, 20min and 30min are respectively sampled and detected in the oil-filled mixing device, and the oil content of insoluble sulfur detection is respectively 18.3%, 21.0% and 23.5%. The physical and chemical indexes of the insoluble sulfur are less destructive, and the oil content index is greatly fluctuated.
Example 6
The procedure of example 3 was used to extend the oil, with the following differences: adjusting the paddle type stirring control rotating speed to 700r/min, keeping other control parameters unchanged, completing the continuous oil filling process, wherein the oil filling speed is as follows: 12 t/h.
The obtained insoluble sulfur product is detected according to GB/T18952-2017, and has an insoluble sulfur content of 97.8% and a thermal stability (105 ℃ 15 min) of 89.7%. 3 time points of discharging for 5min, 20min and 30min are respectively sampled and detected in the oil-filled mixing device, and the oil content of insoluble sulfur detection is respectively 20.0%, 20.0% and 20.0%. The physicochemical index and oil content index of insoluble sulfur are unchanged.
Example 7
The procedure of example 3 was used to extend the oil, with the following differences: the air pressure with nitrogen gas circulation cooling sets up to 0.01MPa, and other control parameters are unchangeable, accomplish continuous oil filling process, oil filling speed: 12 t/h.
The obtained insoluble sulfur product is detected according to GB/T18952-2017, and has an insoluble sulfur content of 97.8% and a thermal stability (105 ℃ 15 min) of 89.7%. 3 time points of discharging for 5min, 20min and 30min are respectively sampled and detected in the oil-filled mixing device, and the oil content in insoluble sulfur detection is respectively 20.5%, 21.6% and 19.1%. Has no influence on the physicochemical indexes of insoluble sulfur, and the oil content index has small fluctuation.
Example 8
The procedure of example 3 was used to extend the oil, with the following differences: the air pressure of the nitrogen circulating cooling is set to be 0.1MPa, other control parameters are unchanged, and the continuous oil filling process is completed. A large amount of materials are accumulated in the oil-filled mixing device, the oil-filled speed is obviously reduced, and the oil-filled speed is as follows: 5 t/h.
The obtained insoluble sulfur product is detected according to GB/T18952-2017, and has an insoluble sulfur content of 97.5% and a thermal stability (105 ℃ 15 min) of 89.6%. 3 time points of discharging for 5min, 20min and 30min are respectively sampled and detected in the oil-filled mixing device, and the oil content of insoluble sulfur detection is respectively 20.0%, 20.0% and 20.0%. Has no influence on physicochemical indexes and oil content indexes of insoluble sulfur.
Example 9
The procedure of example 3 was used to extend the oil, with the following differences: the cloth dish sets up rotational speed 20r/min, and other control parameters are unchangeable, accomplish continuous oil filling process, oil filling speed: 11 t/h.
The obtained insoluble sulfur product is detected according to GB/T18952-2017, and has an insoluble sulfur content of 97.8% and a thermal stability (105 ℃ 15 min) of 89.4%. 3 time points of discharging for 5min, 20min and 30min are respectively sampled and detected in the oil-filled mixing device, and the oil content of insoluble sulfur detection is respectively 19.9%, 20.0% and 20.3%. Has no influence on the physicochemical indexes of insoluble sulfur, and the oil content index has small fluctuation.
Example 10
The procedure of example 3 was used to extend the oil, with the following differences: the cloth dish sets up rotational speed 100r/min, and other control parameters are unchangeable, accomplish continuous oil filling process, oil filling speed: 12 t/h.
The obtained insoluble sulfur product is detected according to GB/T18952-2017, and has an insoluble sulfur content of 97.5% and a thermal stability (105 ℃ 15 min) of 89.9%. 3 time points of discharging for 5min, 20min and 30min are respectively sampled and detected in the oil-filled mixing device, and the oil content of insoluble sulfur detection is respectively 20.0%, 20.0% and 20.0%. Has no influence on physicochemical indexes and oil content indexes of insoluble sulfur.
Example 11
Using the apparatus of example 2, otherwise as in example 3, the oil fill rate: 12 t/h. The obtained insoluble sulfur product is detected according to GB/T18952-2017, the insoluble sulfur content is 97.1%, and the thermal stability (105 ℃ 15 min) is 87.9%. 3 time points of discharging for 5min, 20min and 30min are respectively sampled and detected in the oil-filled mixing device, and the oil content of insoluble sulfur detection is respectively 20.0%, 20.0% and 20.0%.
Comparative example 1
By adopting an intermittent oil filling process, the insoluble sulfur dry powder and the mineral oil which are the same as those in the example 3 are put into a 10-square spiral ribbon mixer according to the ratio of 8:2, the mixture is respectively stirred for 10 minutes, 30 minutes and 50 minutes, 3 samples are taken at different positions of the mixer, the oil content of the product is detected, and simultaneously the quality of the insoluble sulfur is detected according to GB/T18952-2017, and the results are shown in the following table 1:
comparative example 2
The procedure of example 3 was used to extend the oil, with the following differences: adjusting the paddle type stirring control rotating speed to 1000r/min, keeping other control parameters unchanged, completing the continuous oil filling process, wherein the oil filling speed is as follows: 12 t/h.
The obtained insoluble sulfur product is detected according to GB/T18952-2017, the insoluble sulfur content is 96.8%, and the thermal stability (105 ℃ 15 min) is 84.2%. 3 time points of discharging for 5min, 20min and 30min are respectively sampled and detected in the oil-filled mixing device, and the oil content of insoluble sulfur detection is respectively 20.0%, 20.0% and 20.0%. The oil content index has good stability, and the physical and chemical indexes of the insoluble sulfur have great destructiveness.
Comparative example 3
An oil-filled mixing device of the same construction as in example 2 was used, except that: wherein, no cloth disc is arranged, and the insoluble sulfur is directly introduced into the kettle body from the dry powder feeding pipe. Oil charge was carried out using the process flow of example 3, oil charge rate: 12 t/h.
The obtained insoluble sulfur product is detected according to GB/T18952-2017, the insoluble sulfur content is 96.9%, and the thermal stability (105 ℃ 15 min) is 86.8%. 3 time points of discharging for 5min, 20min and 30min are respectively sampled and detected in the oil-filled mixing device, and the oil content of insoluble sulfur detection is 14.2%, 19.5% and 20.5% respectively. The oil content index has large fluctuation and the mixing effect is not good.
Claims (10)
1. A continuous oil filling method of insoluble sulfur is characterized by comprising the following steps:
(1) the insoluble sulfur dry powder continuously falls onto a material distribution disc rotating in an oil-filled mixing device through a dry powder feeding pipe, and the insoluble sulfur dry powder continuously falls into the bottom of the oil-filled mixing device along the edge of the material distribution disc under the drive of the material distribution disc;
(2) continuously spraying mineral oil into an oil-filled mixing device in a spraying mode while adding the insoluble sulfur dry powder, so that the insoluble sulfur dry powder is fully mixed with mineral oil spray in the falling process;
(3) and discharging the insoluble sulfur and the mineral oil which are uniformly mixed at the bottom of the oil-filled mixing device from a discharge hole.
2. The continuous oil-filling method according to claim 1, wherein: the rotating speed of the cloth disc is 20-100r/min, preferably 40 r/min.
3. The continuous oil-filling method according to claim 1 or 2, characterized in that: the small droplets in mineral oil sprays have a particle size in the range of 1 to 100. mu.m, preferably 30 to 50 μm.
4. The continuous oil-filling method according to claim 1 or 2, characterized in that: the feeding speed of the insoluble sulfur dry powder is 140-160kg/min, and the mass ratio of the feeding amount of the insoluble sulfur to the feeding amount of the mineral oil in unit time is 8: 2.
5. The continuous oil-filling method according to any one of claims 1 to 4, characterized in that: in the step (2), the insoluble sulfur is subjected to high-speed shearing in the falling process, the shearing speed is 400-; preferably, in the step (2), circulating cold air flows from the bottom of the kettle to the top of the kettle in the oil-filled mixing device, the temperature of the circulating cold air is 20-35 ℃, and the air pressure is 0.01-0.1 MPa, preferably 0.04 MPa.
6. The utility model provides an oil charge mixing arrangement of insoluble sulphur, includes the cauldron body, characterized by: the material distribution structure is arranged in the kettle body, is positioned at the upper part of the kettle body and comprises a motor positioned at the top of the kettle body, the output end of the motor is connected with a stirring rod, the tail end of the stirring rod is connected with a horizontally arranged material distribution plate, the upper part of the kettle body is provided with a dry powder feeding pipe, and the outlet of the feeding pipe is positioned above the material distribution plate to ensure that the insoluble sulfur dry powder falls onto the material distribution plate; still be equipped with a plurality of mineral oil inlet pipes on the cauldron body lateral wall, the export of every mineral oil inlet pipe all is connected with atomizer, atomizer is located the below of cloth dish, and atomizer uses cloth dish to enclose into the diameter of a circle that circular and atomizer formed as the axle center and is greater than cloth dish diameter, and each atomizer's material blowout direction is perpendicular with the decline direction of insoluble sulphur.
7. The oil-filled mixing device of claim 6, wherein: the cloth disc is a circular flat plate, and micropores are uniformly formed in the cloth disc; preferably, the ratio of the diameter of the material distribution disc to the diameter of the kettle body is 2-6:10, preferably 4: 10.
8. the oil-filled mixing device of claim 6, wherein: the number of the atomizing nozzles is more than or equal to 2, preferably 4; preferably, the atomizing nozzles are located on the same horizontal plane, and the intervals between the atomizing nozzles are the same.
9. The oil-filled mixing device of claim 6, wherein: a high-speed shearing structure is arranged at the lower part of the kettle body, and the high-speed shearing structure comprises at least one stirrer, preferably 3 stirrers; preferably, the stirrer is a paddle stirrer, a propeller stirrer or an anchor stirrer.
10. The oil-filled mixing device according to claim 6 or 9, wherein: a heat-insulating jacket or a cold air circulating system is also arranged on the kettle body, the cold air circulating system comprises an air inlet pipe and an air outlet pipe, one end of the air inlet pipe is positioned in the kettle body, the other end of the air inlet pipe is connected with a fan, one end of the air outlet pipe is connected with an air outlet at the top of the kettle body, the other end of the air outlet pipe is connected with the fan, and a condenser is also arranged between the air inlet pipe and the fan; preferably, the bottom of the kettle body is provided with a discharge port, the discharge port is connected with a continuous conveying device in a sealing manner, and the continuous conveying device is preferably a double-shaft screw conveyor.
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| CN116550202A (en) * | 2023-05-23 | 2023-08-08 | 广州市来力实业有限公司 | Vulcanizing agent production process |
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| CN114100473B (en) | 2024-05-17 |
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