CN114100473B - 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
- Publication number
- CN114100473B CN114100473B CN202111361440.6A CN202111361440A CN114100473B CN 114100473 B CN114100473 B CN 114100473B CN 202111361440 A CN202111361440 A CN 202111361440A CN 114100473 B CN114100473 B CN 114100473B
- Authority
- CN
- China
- Prior art keywords
- oil
- insoluble sulfur
- mixing device
- kettle body
- dry powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 142
- 239000011593 sulfur Substances 0.000 title claims abstract description 115
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 115
- 238000002156 mixing Methods 0.000 title claims abstract description 74
- 238000011049 filling Methods 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 36
- 239000003921 oil Substances 0.000 claims abstract description 156
- 239000000843 powder Substances 0.000 claims abstract description 54
- 239000002480 mineral oil Substances 0.000 claims abstract description 52
- 235000010446 mineral oil Nutrition 0.000 claims abstract description 52
- 238000005429 filling process Methods 0.000 claims abstract description 20
- 238000007599 discharging Methods 0.000 claims abstract description 14
- 239000007921 spray Substances 0.000 claims abstract description 12
- 238000005507 spraying Methods 0.000 claims abstract description 9
- 238000009826 distribution Methods 0.000 claims description 41
- 239000000463 material Substances 0.000 claims description 39
- 239000004744 fabric Substances 0.000 claims description 14
- 238000010008 shearing Methods 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 10
- 238000000889 atomisation Methods 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 239000005864 Sulphur Substances 0.000 description 25
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 24
- 229910052757 nitrogen Inorganic materials 0.000 description 12
- 238000005070 sampling Methods 0.000 description 11
- 239000000126 substance Substances 0.000 description 8
- 239000007789 gas Substances 0.000 description 7
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 238000004321 preservation Methods 0.000 description 5
- 238000004806 packaging method and process Methods 0.000 description 4
- 239000000725 suspension Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000004033 diameter control Methods 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 238000010057 rubber processing Methods 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
- Mixers Of The Rotary Stirring Type (AREA)
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: continuously dropping insoluble sulfur dry powder onto a rotating distributing disc in an oil-filled mixing device through a feeding pipe, wherein the insoluble sulfur dry powder continuously drops into the bottom of the device along the edge of the distributing disc; continuously spraying mineral oil in a spray mode while adding insoluble sulfur dry powder, so that the insoluble sulfur is fully mixed with mineral oil in a falling process; and discharging the insoluble sulfur and mineral oil which are uniformly mixed at the bottom of the device through a discharge port. According to the invention, insoluble sulfur is dispersed in a mixing device in a distributing disc manner, mineral oil is contacted with the insoluble sulfur in an atomizing manner, and the oil filling process is completed instantaneously, so that the production efficiency is remarkably improved. According to the invention, the oil filling process is finished instantaneously, the mineral oil and the insoluble sulfur are uniformly contacted and mixed, the oil filling time is greatly shortened, the influence on the content of the insoluble sulfur and the thermal stability is reduced to the greatest extent, and the product quality is improved.
Description
Technical Field
The invention relates to a continuous oil filling method of 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 with excellent performance, and can be classified into an oil-filled type and a non-oil-filled type according to whether oil is filled in the post-treatment process. Because of the defects of small particle size, easy flying, large dust, difficult dispersion during mixing, inflammability and explosiveness and the like of the non-oil-filled insoluble sulfur, the oil-filled insoluble sulfur is commonly used in rubber processing and tire industries.
At present, the preparation of oil-filled insoluble sulfur mainly adopts an intermittent production process, which is simply described as follows: the insoluble sulfur dry powder and mineral oil are put into a mixer according to a certain proportion for one time, stirred for a certain time, and whether the oil content is qualified or not is detected, discharged and packaged. Because of large feeding amount and long mixing time, the thermal stability and content of insoluble sulfur are reduced, and the insoluble sulfur is one of important factors affecting the quality of products. Therefore, insoluble sulfur manufacturers continually explore and innovate, and find new oil filling modes.
An oil filling device for insoluble sulphur is disclosed in chinese patent CN 204134500U, for example, which uses an auger to fill the oil. The wall of the spiral propeller is provided with a plurality of oil filling ports, insoluble sulfur moves along the axial direction of the rotating shaft under the pushing of the spiral blades and is stirred by the spiral blades, and the insoluble sulfur can sequentially contact and mix with oil entering through the oil filling ports along with the movement of the insoluble sulfur, so that the aim of continuously filling oil is fulfilled. However, the spiral blade has axial pushing effect, the shearing force is small, and the uniform mixing of insoluble sulfur and oil products cannot be ensured.
Chinese patent CN 10820381a discloses a method and apparatus for producing oil-filled insoluble sulfur, in which, in the desolventizing step, powdered insoluble sulfur which is not completely desolventized is heated together with mineral oil, so that carbon disulfide remaining in the powdered insoluble sulfur which is not completely desolventized is dissolved in the mineral oil and escapes, thereby achieving the effect of complete desolventizing. Because the carbon disulfide has certain solubility in mineral oil, the desolventizing time is relatively long, and the physical and chemical indexes of insoluble sulfur are influenced to a certain extent.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention provides a continuous oil filling method of insoluble sulfur, which continuously enters insoluble sulfur dry powder into a mixing device, and mineral oil is mixed by spraying, so that the two are mixed uniformly in the moment, the operation time is obviously shortened by finishing oil filling in the moment, the production efficiency of the oil filling process is improved, the influence of the mixing process on the heat 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, comprising the following steps:
(1) Continuously dropping insoluble sulfur dry powder onto a material distribution plate rotating in the oil-filled mixing device through a dry powder feeding pipe, and continuously dropping the insoluble sulfur dry powder into the bottom of the oil-filled mixing device along the edge of the material distribution plate under the drive of the material distribution plate;
(2) Continuously spraying mineral oil into an oil-filled mixing device in a spraying mode while adding insoluble sulfur dry powder, so that the insoluble sulfur dry powder is fully mixed with mineral oil in a spraying mode in the falling process;
(3) And discharging the insoluble sulfur and mineral oil which are uniformly mixed at the bottom of the oil-filled mixing device from a discharge port.
In the method, the insoluble sulfur dry powder and the mineral oil are respectively and accurately conveyed into the oil-filled mixing device by a continuous conveying device with a metering and adjusting function in proportion, and the feeding metering equipment of the insoluble sulfur dry powder can be a weightless feeding scale, a powder material quantitative feeder, a solid material flowmeter (comprising a chute type and impulse type), a rotor scale (comprising a Phillips type, a powder grinding type and the like), a Coriolis mass flowmeter, a spiral scale, a powder material nucleon scale and the like, and is preferably a weightless feeding scale.
Further, the feeding speed of the insoluble sulfur dry powder is 140-160kg/min, and the mass ratio of the insoluble sulfur to the mineral oil in unit time is about 8:2. In this range, the insoluble sulfur dry powder can be better mixed with the atomized mineral oil during the falling process.
Further, the mineral oil is a white oil or a naphthenic oil.
Further, the size of the droplets in the mineral oil spray is in the range of 1 to 100. Mu.m, preferably 30 to 50. Mu.m. The atomization of the mineral oil may be achieved in the manner commonly used today, for example by means of atomizers, for example by means of pressurizing means, which may be a pressurizing pump, gas pressurizing or the like.
Further, the rotating speed of the distribution plate is 20-100r/min, preferably 40r/min. After insoluble sulfur dry powder falls into the cloth dish, can make insoluble sulfur dry powder evenly distributed on the cloth dish through rotatory to along with insoluble sulfur dry powder's increase, it can evenly fall along the edge of cloth dish, in the in-process that falls, insoluble sulfur dry powder is cylindrical, has formed a columniform curtain, and mineral oil distributes in oil filling mixing arrangement in the form of droplet, evenly sprays the surface at the curtain at insoluble sulfur in-process that falls, has realized mineral oil and insoluble sulfur's even mixing in the twinkling of an eye. 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 distribution disc to the oil-filled mixing device is 2:10-6:10, preferably 4:10. the diameter setting is matched with the rotating speed, the feeding speed of the materials and the particle size of mineral oil, so that the effect is better.
Furthermore, the invention also provides a preferable mode, wherein the bottom of the oil-filled mixing device is also provided with a high-speed shearing structure, materials can be scattered when falling onto the high-speed shearing structure, the mixing is more uniform, and the shearing speed is 400-1000r/min, preferably 700-800r/min. The mixing effect is further improved by adding the stirring step.
Furthermore, the invention also provides a preferable mode, wherein a cold air circulation system is further arranged in the oil-filled mixing device, and the cold air circulation system is started from the addition of 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 air pressure of the circulating cold air is 0.01MPa-0.1MPa, preferably 0.04MPa, the temperature of the oil-filled mixing device at each position can be kept at 20 ℃ -35 ℃ (preferably 20-25 ℃), the insoluble sulfur dry powder can be ensured to be in a suspension state, and the oil-filled mixing device is more convenient to mix with mineral oil. Compared with heat preservation structures such as a heat preservation jacket, the cold air circulation system can better realize the constancy of temperature in the oil-filled mixing device, improve the heat exchange efficiency, and better promote the quality of insoluble sulfur. The cold air circulation system can be used simultaneously with a high-speed shearing structure, and also can be used independently.
Furthermore, the whole oil-filled mixing process is performed in a nitrogen environment, and the safety of the whole process can be improved due to the existence of nitrogen. For example, mineral oil sprays use nitrogen as a carrier, and nitrogen is circulated in an oil-filled mixing device in a cold air circulation system, and the like.
Further, the cold air circulation system keeps the pressure of circulating nitrogen in the oil-filled mixing device at 0.01MPa-0.1MPa, preferably 0.04MPa. 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.
Further, 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, so that the oil-filled mixing device is not emptied during discharging, and a part of the mixture of the insoluble sulfur and the mineral oil always exists in the kettle.
The invention also provides an oil-filled mixing device for continuous oil-filled of insoluble sulfur, which 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 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 to ensure that 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 the cloth dish as the axle center to enclose into a circular and atomizer formed circle's diameter is greater than cloth dish diameter, and the material blowout direction of each atomizer is perpendicular with insoluble sulphur's decline direction.
Further, the distribution plate is a circular flat plate, micropores are uniformly formed in the circular flat plate, and the circular flat plate is hollowed out, so that insoluble sulfur is prevented from adhering to the upper surface of the distribution plate. The micropores ensure that insoluble sulfur cannot fall off.
Preferably, the outlet of the dry powder feeding pipe is positioned right above the distributing plate, or a flow dividing plate can be further arranged on the distributing plate, so that the uniform distribution of insoluble sulfur dry powder on the distributing plate is better ensured.
Further, the diameter control ratio of the distribution disc to the oil-filled mixing device is 2:10-6:10, preferably 4:10.
Further, the number of the atomizing nozzles is greater than or equal to 2, preferably 4, that is, the number of the mineral oil feeding pipes is greater 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 spray, preferably 4. Each atomizing nozzle is positioned on the same horizontal plane to form a circle and is positioned below the distribution plate, and the intervals among the atomizing nozzles are the same.
Further, the atomization of the mineral oil can be achieved by installing a pressurizing device in front of the atomization nozzle and on the mineral oil feeding pipe, wherein the pressurizing device can be a pressurizing pump, a gas pressurizing device and the like, and is preferably a nitrogen pressurizing device.
Further, the lower part in the cauldron body is equipped with high-speed shearing structure, high-speed shearing structure is located the lower part of the cauldron body, and atomizer's below cuts the material that falls on it and breaks up, and high-speed shearing structure includes at least one agitator. The stirrers are arranged on the side wall of the kettle body, and the stirrers are preferably uniformly distributed. The number of agitators ensures that the material falling from the upper part is sheared sufficiently, preferably 3 agitators.
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.
Further, a heat preservation jacket or a cold air circulation system is arranged on the kettle body and used for maintaining the temperature of the kettle body. The cold air circulation system comprises an air inlet pipe and an air outlet pipe, wherein the air inlet pipe enters the lower part of the kettle body through an air inlet on 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 at 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 a required temperature and then is discharged into the kettle body. The gas enters from the bottom of the kettle body, is discharged from the top, and the flowing direction and certain pressure of the circulating gas strengthen the dispersion and suspension of insoluble sulfur.
Further, a discharge hole is formed in the bottom of the kettle body and is in sealing connection with a continuous conveying device, and the continuous conveying device is preferably a double-shaft screw conveyor. The continuous conveying device continuously conveys the mixed oil powder to downstream packaging equipment, so that the oil filling process is completed.
The invention has the following beneficial effects:
1. according to the invention, insoluble sulfur is dispersed in a mixing device in a distributing disc manner, mineral oil is contacted with the insoluble sulfur in an atomizing manner, and the oil filling process is completed instantaneously, so that the production efficiency is remarkably improved.
2. According to the invention, the oil filling process is finished instantaneously, the mineral oil and the insoluble sulfur are uniformly contacted and mixed, the oil filling time is greatly shortened, the influence on the content of the insoluble sulfur and the thermal stability is reduced to the greatest extent, and the product quality is improved.
3. According to the invention, the mixing device is improved, the distribution plate, the atomizing nozzle and the cold air circulation system are added, so that the contact efficiency and the heat transfer efficiency of insoluble sulfur and mineral oil are greatly improved, and the production efficiency and the quality of insoluble sulfur are improved.
Drawings
FIG. 1 is a schematic diagram of the oil-filled mixing device for insoluble sulfur according to the present invention.
In the figure, 1, a dry powder feeding pipe; 2. a cloth tray; 3. a mineral oil feed tube; 4. a condenser; 5. an atomizing nozzle; 6. a high speed shear structure; 7. a blower; 8. a continuous conveying device.
Detailed Description
The present invention will be described in further detail with reference to the following examples. These specific examples are intended to be illustrative of the invention and are not intended to be limiting.
Example 1
As shown in figure 1, the oil-filled mixing device of insoluble sulfur with a preferred structure comprises a kettle body, wherein the kettle body is provided with a hollow cavity, a material distribution structure is arranged in the kettle body and positioned at the upper part of the kettle body, the oil-filled mixing device 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 material distribution plate is a circular flat plate, micropores are uniformly arranged on the material distribution plate and are hollow, and insoluble sulfur cannot fall 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 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 a circular shape and the diameter of the circle that atomizer formed is greater than cloth dish diameter as the axle center, and the material blowout direction of each atomizer is perpendicular with insoluble sulphur's decline direction. The number of the atomizing nozzles is more than or equal to 2, preferably 4, so that all falling insoluble sulfur can be fully contacted and mixed with the spray by the sprayed mineral oil.
The lower part in the kettle body is also provided with a high-speed shearing structure which 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, a propeller stirrer, an anchor stirrer or the like, preferably a paddle stirrer, for example a paddle stirrer.
And a cold air circulation system is also arranged on the kettle body and is used for maintaining the temperature of the kettle body. The cold air circulation system comprises an air inlet pipe and an air outlet pipe, wherein the air inlet pipe enters the lower part of the kettle body through an air inlet on the kettle body, air exhausted from the air inlet pipe flows along 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, the other end of the air inlet pipe is connected with a fan, the air outlet pipe is connected with an air outlet at the top of the kettle, 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 from the fan is cooled to the required temperature and then discharged into the kettle. The 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 nitrogen is circulated in the cold air circulation system.
The bottom of the kettle body is provided with a discharge hole, the discharge hole is connected with a continuous conveying device in a sealing way, and the continuous conveying device is preferably a double-shaft screw conveyor. The continuous conveying device continuously conveys the mixed oil powder to downstream packaging equipment, so that the oil filling process is completed.
The process for realizing continuous oil filling by adopting the oil filling mixing device comprises the following steps:
1. Continuously conveying insoluble sulfur dry powder and mineral oil into an oil-filled mixing device according to a proportion;
2. The insoluble sulfur dry powder enters an oil-filled mixing device and falls on a distribution plate by gravity, and in the process of uniform rotation of the distribution plate, the dry powder forms a stable cylindrical material curtain at the edge of the distribution plate and falls at a uniform speed;
3. The mineral oil is sprayed out in the form of small liquid drops through the atomizing spray heads 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 nozzle ensure that the insoluble sulfur dry powder and mineral oil are instantaneously and uniformly mixed, and meanwhile, the temperature of the materials is not obviously changed.
5. The oil powder after being fully and uniformly mixed is conveyed to downstream packaging equipment by the continuous conveying device, and is further stirred in the conveying process, so that the oil powder is further mixed, and meanwhile, mineral oil enters the powder from the surface of the insoluble sulfur powder, so that the stability of the oil content can be further ensured.
Example 2
The structure of the oil-filled mixing device for insoluble sulfur is the same as that of example 1, except that: the kettle does not contain a cold air circulation system, but is provided with a heat preservation jacket outside the kettle body, and flowing condensed water or condensed oil is arranged in the heat preservation jacket and used for keeping the temperature.
Example 3
The oil-filled mixing device with the volume of 8 cubic is selected, the structure is the same as that of the embodiment 1, and the ratio of the diameter of the distributing disc to the diameter of the kettle body is 4:10. adding insoluble sulfur dry powder into an oil-filled mixing device through a weightlessness scale, wherein the feeding speed is 160kg/min. The dry powder falls onto the surface of a material distribution plate by gravity, the material distribution plate is provided with a rotating speed of 40r/min, and the dry powder forms a stable cylindrical material curtain at the edge of the material distribution plate 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 size of small liquid drops of the naphthenic oil is 30-50 mu m, and the total feeding speed of the naphthenic oil is 40kg/min. And 3 paddle stirrers are uniformly arranged below the atomizing nozzle, the rotating speed is controlled to be 800r/min, meanwhile, the cold air circulation system is controlled to operate, the air pressure of nitrogen circulation is ensured to be 0.04MPa, and the temperature is 25 ℃. The oil-filled powder falling to the bottom is transferred to downstream packaging equipment through a double-shaft screw conveyor to complete the continuous oil-filling process, the discharge ensures that the oil-filling mixing device is not empty in a kettle, and the oil-filling rate is high: 12 tons/h.
The insoluble sulphur product obtained was tested according to GB/T18952-2017, the insoluble sulphur content was 97.8%, the thermal stability (105 ℃ C. For 15 min) was 89.7%. And the oil is discharged from the oil-filled mixing device for 5min,20min and 30min for 3 time points for sampling detection, the oil content of the insoluble sulfur is 20.0%, 20.0% and 20.0% respectively, and the oil content index has good stability.
Example 4
The process flow of example 3 was used for oil filling, with the difference that: the number of the atomizing spray heads is set to 3, the continuous oil filling process is completed, and the oil filling rate is increased: 12t/h.
The insoluble sulphur product obtained was tested according to GB/T18952-2017, the insoluble sulphur content was 97.1%, the thermal stability (105 ℃ C. For 15 min) was 89.2%. Sampling and detecting are carried out at 5min,20min and 30min3 time points of discharging of the oil-filled mixing device, the oil content of insoluble sulfur is respectively 20.0%, 21.0% and 19.5%, and the oil content index has smaller fluctuation.
Example 5
The process flow of example 3 was used for oil filling, with the difference that: the paddle type stirring control rotating speed is adjusted to 400r/min, other control parameters are unchanged, the continuous oil filling process is completed, and the oil filling rate is increased: 12t/h.
The insoluble sulphur product obtained was tested according to GB/T18952-2017, the insoluble sulphur content was 97.6%, the thermal stability (105 ℃ C. For 15 min) was 89.6%. Sampling and detecting are carried out at 5min,20min and 30min3 time points of discharging of the oil-filled mixing device, and the oil content of insoluble sulfur is 18.3%, 21.0% and 23.5% respectively. The insoluble sulfur physical and chemical indexes have small destructiveness, and the oil content indexes have larger fluctuation.
Example 6
The process flow of example 3 was used for oil filling, with the difference that: the paddle type stirring control rotating speed is adjusted to 700r/min, other control parameters are unchanged, the continuous oil filling process is completed, and the oil filling rate is increased: 12t/h.
The insoluble sulphur product obtained was tested according to GB/T18952-2017, the insoluble sulphur content was 97.8%, the thermal stability (105 ℃ C. For 15 min) was 89.7%. Sampling and detecting are carried out at 5min,20min and 30min3 time points of discharging of the oil-filled mixing device, and the oil content of insoluble sulfur is 20.0%, 20.0% and 20.0% respectively. The physical and chemical indexes and the oil content indexes of the insoluble sulfur are unchanged.
Example 7
The process flow of example 3 was used for oil filling, with the difference that: the air pressure of nitrogen circulating cooling is set to be 0.01MPa, other control parameters are unchanged, the continuous oil filling process is completed, and the oil filling rate is increased: 12t/h.
The insoluble sulphur product obtained was tested according to GB/T18952-2017, the insoluble sulphur content was 97.8%, the thermal stability (105 ℃ C. For 15 min) was 89.7%. Sampling and detecting are carried out at 5min,20min and 30min3 time points of discharging of the oil-filled mixing device, and the oil content of insoluble sulfur is 20.5%, 21.6% and 19.1% respectively. Has no influence on the physical and chemical indexes of insoluble sulfur, and the oil content index has small fluctuation.
Example 8
The process flow of example 3 was used for oil filling, with the difference that: and setting the air pressure of nitrogen circulating cooling to be 0.1MPa, and completing the continuous oil filling process without changing other control parameters. A large amount of materials are piled up in the oil-filled mixing device, the oil-filled rate is obviously reduced, and the oil-filled rate is: 5t/h.
The insoluble sulphur product obtained was tested according to GB/T18952-2017, the insoluble sulphur content was 97.5%, the thermal stability (105 ℃ C. For 15 min) was 89.6%. Sampling and detecting are carried out at 5min,20min and 30min3 time points of discharging of the oil-filled mixing device, and the oil content of insoluble sulfur is 20.0%, 20.0% and 20.0% respectively. Has no influence on insoluble sulfur physical and chemical indexes and oil content indexes.
Example 9
The process flow of example 3 was used for oil filling, with the difference that: the rotating speed of the cloth disc is set to 20r/min, other control parameters are unchanged, the continuous oil filling process is completed, and the oil filling rate is increased: 11t/h.
The insoluble sulphur product obtained was tested according to GB/T18952-2017, the insoluble sulphur content was 97.8%, the thermal stability (105 ℃ C. For 15 min) was 89.4%. Sampling and detecting are carried out at 5min,20min and 30min3 time points of discharging of the oil-filled mixing device, and the oil content of insoluble sulfur is 19.9%, 20.0% and 20.3% respectively. Has no influence on the physical and chemical indexes of insoluble sulfur, and the oil content index has small fluctuation.
Example 10
The process flow of example 3 was used for oil filling, with the difference that: the rotating speed of the cloth disc is set to 100r/min, other control parameters are unchanged, the continuous oil filling process is completed, and the oil filling rate is increased: 12t/h.
The insoluble sulphur product obtained was tested according to GB/T18952-2017, the insoluble sulphur content was 97.5%, the thermal stability (105 ℃ C. For 15 min) was 89.9%. Sampling and detecting are carried out at 5min,20min and 30min3 time points of discharging of the oil-filled mixing device, and the oil content of insoluble sulfur is 20.0%, 20.0% and 20.0% respectively. Has no influence on insoluble sulfur physical and chemical indexes and oil content indexes.
Example 11
Using the apparatus of example 2, the oil charge rate was otherwise the same as example 3: 12t/h. The insoluble sulphur product obtained was tested according to GB/T18952-2017, and had an insoluble sulphur content of 97.1% and a thermal stability (105 ℃ C. For 15 min) of 87.9%. Sampling and detecting are carried out at 5min,20min and 30min3 time points of discharging of the oil-filled mixing device, and the oil content of insoluble sulfur is 20.0%, 20.0% and 20.0% respectively.
Comparative example 1
The same insoluble sulfur dry powder and mineral oil as in example 3 were put into a 10-side ribbon mixer in a ratio of 8:2 by using an intermittent oil charging process, and stirred for 10 minutes, 30 minutes and 50 minutes, respectively, 3 samples were taken at different positions of the mixer, and the oil content of the product was detected, and at the same time, the quality of insoluble sulfur was detected according to GB/T18952-2017, and the results are shown in Table 1 below:
Comparative example 2
The process flow of example 3 was used for oil filling, with the difference that: the paddle type stirring control rotating speed is adjusted to 1000r/min, other control parameters are unchanged, the continuous oil filling process is completed, and the oil filling rate is increased: 12t/h.
The insoluble sulphur product obtained was tested according to GB/T18952-2017, with an insoluble sulphur content of 96.8% and a thermal stability (105 ℃ C. For 15 min) of 84.2%. Sampling and detecting are carried out at 5min,20min and 30min3 time points of discharging of the oil-filled mixing device, and the oil content of insoluble sulfur is 20.0%, 20.0% and 20.0% respectively. The oil content index has good stability and the insoluble sulfur physical and chemical index has large destructiveness.
Comparative example 3
The same oil-filled mixing device as in example 2 was used, except that: wherein, a distributing disc is not arranged, and insoluble sulfur is directly introduced into the kettle body from a dry powder feeding pipe. Oil charge was performed using the process flow of example 3, oil charge rate: 12t/h.
The insoluble sulphur product obtained was tested according to GB/T18952-2017, with an insoluble sulphur content of 96.9% and a thermal stability (105 ℃ C. For 15 min) of 86.8%. Sampling and detecting are carried out at 5min,20min and 30min3 time points of discharging of the oil-filled mixing device, and the oil content of insoluble sulfur is 14.2%, 19.5% and 20.5% respectively. The oil content index fluctuates greatly, and the mixing effect is poor.
Claims (12)
1. The continuous oil filling method of insoluble sulfur is characterized by comprising the following steps:
(1) Continuously dropping insoluble sulfur dry powder onto a material distribution plate rotating in the oil-filled mixing device through a dry powder feeding pipe, and continuously dropping the insoluble sulfur dry powder into the bottom of the oil-filled mixing device along the edge of the material distribution plate under the drive of the material distribution plate;
(2) Continuously spraying mineral oil into an oil-filled mixing device in a spraying mode while adding insoluble sulfur dry powder, so that the insoluble sulfur dry powder is fully mixed with mineral oil in a spraying mode in the falling process;
(3) Discharging insoluble sulfur and mineral oil which are uniformly mixed at the bottom of the oil-filled mixing device from a discharge port;
the distribution plate is a circular flat plate, and micropores are uniformly formed in the distribution plate;
the rotating speed of the cloth disc is 20-100r/min;
the particle size of the small liquid drops in the mineral oil spray is 1-100 mu m;
In the step (2), insoluble sulfur is sheared at a high speed in the falling process, and the shearing speed is 400-1000r/min;
In the step (2), the oil-filled mixing device is provided with circulating cold air in the flowing direction from the bottom of the kettle to the top of the kettle, wherein the temperature of the circulating cold air is 20-35 ℃ and the wind pressure is 0.01-0.1 MPa.
2. The continuous oil-filling process according to claim 1, characterized in that: the rotating speed of the cloth disc is 40r/min.
3. The continuous oil-filling process according to claim 1 or 2, characterized in that: the size of the droplets in the mineral oil spray is in the range of 30-50 μm.
4. The continuous oil-filling process 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 insoluble sulfur to the mineral oil in unit time is 8:2.
5. The continuous oil-filling process according to claim 1 or 2, characterized in that: in the step (2), insoluble sulfur is sheared at a high speed in the falling process, and the shearing speed is 700-800r/min; in the step (2), the air pressure of the circulating cold air is 0.04Mpa.
6. The utility model provides an insoluble sulfur's oil charge mixing arrangement, includes the cauldron body, characterized by: the kettle body is internally provided with a material distribution structure, 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 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 disc to ensure that insoluble dry sulfur powder falls onto the material distribution disc; the side wall of the kettle body is also provided with a plurality of mineral oil feeding pipes, an outlet of each mineral oil feeding pipe is connected with an atomization nozzle, the atomization nozzle is positioned below the distribution plate, the atomization nozzle surrounds the distribution plate as an axis to form a circle, the diameter of the circle formed by the atomization nozzle is larger than that of the distribution plate, and the material spraying direction of each atomization nozzle is perpendicular to the descending direction of insoluble sulfur; the distribution plate is a circular flat plate, micropores are uniformly formed on the distribution plate, and the ratio of the diameter of the distribution plate to the diameter of the kettle body is 2-6:10; the lower part of the kettle body is provided with a high-speed shearing structure which comprises at least one stirrer; the kettle body is also provided with a cold air circulation system, the cold air circulation 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 arranged between the air inlet pipe and the fan; the bottom of the kettle body is provided with a discharge hole, the discharge hole is connected with a continuous conveying device in a sealing way, and the continuous conveying device is a double-shaft screw conveyor.
7. The oil-filled mixing device of claim 6, wherein: the ratio of the diameter of the distributing disc to the diameter of the kettle body is 4:10.
8. The oil-filled mixing device of claim 6, wherein: the number of the atomizing spray heads is more than or equal to 2.
9. The oil-filled mixing device of claim 8, wherein: the number of the atomizing spray heads is 4.
10. The oil-filled mixing device of claim 6, wherein: the atomizing nozzles are positioned on the same horizontal plane, and the intervals among the atomizing nozzles are the same.
11. The oil-filled mixing device of claim 6, wherein: the high speed shear structure includes 3 agitators.
12. The oil-filled mixing device of claim 6, wherein: the stirrer is a paddle stirrer, a propeller stirrer or an anchor stirrer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111361440.6A CN114100473B (en) | 2021-11-17 | 2021-11-17 | Continuous oil filling method and oil filling mixing device for insoluble sulfur |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111361440.6A CN114100473B (en) | 2021-11-17 | 2021-11-17 | Continuous oil filling method and oil filling mixing device for insoluble sulfur |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114100473A CN114100473A (en) | 2022-03-01 |
| CN114100473B true CN114100473B (en) | 2024-05-17 |
Family
ID=80396107
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111361440.6A Active CN114100473B (en) | 2021-11-17 | 2021-11-17 | Continuous oil filling method and oil filling mixing device for insoluble sulfur |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114100473B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116550202B (en) * | 2023-05-23 | 2023-10-27 | 广州市来力实业有限公司 | Vulcanizing agent production process |
Citations (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3979316A (en) * | 1972-09-27 | 1976-09-07 | Kali-Chemie Aktiengesellschaft | Pelleted sulfur compositions and processes for their production |
| SU715449A1 (en) * | 1978-09-04 | 1980-02-15 | Предприятие П/Я А-3326 | Method of producing insoluble sulfure |
| JP2005185903A (en) * | 2003-12-24 | 2005-07-14 | Naris Cosmetics Co Ltd | Oil spray installation for powder |
| CN101037191A (en) * | 2007-03-20 | 2007-09-19 | 南京工业大学 | Preparation method of oil-filled insoluble sulphur |
| CN203568846U (en) * | 2013-10-12 | 2014-04-30 | 江苏宏泰橡胶助剂有限公司 | Device for preparing high-quality insoluble sulphur |
| CN208265778U (en) * | 2018-03-19 | 2018-12-21 | 无锡华盛橡胶新材料科技股份有限公司 | A kind of production equipment of oil-filled insoluble sulfur |
| CN109126602A (en) * | 2018-09-18 | 2019-01-04 | 北京燕山粉研精机有限公司 | Powder liquid continuous mixer and continuous metering mixture manufacturing line |
| CN210131550U (en) * | 2019-05-22 | 2020-03-10 | 宜昌阿波罗肥业有限公司 | Compound fertilizer material adjusting device |
| CN111547684A (en) * | 2020-05-13 | 2020-08-18 | 山东润初企业管理咨询有限责任公司 | Production method of insoluble sulfur and insoluble sulfur |
| CN211636311U (en) * | 2019-08-17 | 2020-10-09 | 青岛凯立德生物科技有限公司 | Fat powder blending device convenient to clean |
| CN212632322U (en) * | 2020-05-18 | 2021-03-02 | 太阳树(莆田)生物医药有限公司 | A blendor for plant draws |
| CN113522074A (en) * | 2020-04-15 | 2021-10-22 | 中国石油化工股份有限公司 | Powder-liquid mixing equipment |
| CN214635879U (en) * | 2020-12-28 | 2021-11-09 | 中原环保郑州污泥新材料科技有限公司 | Mixing arrangement is used in flocculating agent production |
| KR20220001936A (en) * | 2020-06-30 | 2022-01-06 | 주식회사 엔티시스템 | Manufacturing method of insoluble sulfur |
-
2021
- 2021-11-17 CN CN202111361440.6A patent/CN114100473B/en active Active
Patent Citations (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3979316A (en) * | 1972-09-27 | 1976-09-07 | Kali-Chemie Aktiengesellschaft | Pelleted sulfur compositions and processes for their production |
| SU715449A1 (en) * | 1978-09-04 | 1980-02-15 | Предприятие П/Я А-3326 | Method of producing insoluble sulfure |
| JP2005185903A (en) * | 2003-12-24 | 2005-07-14 | Naris Cosmetics Co Ltd | Oil spray installation for powder |
| CN101037191A (en) * | 2007-03-20 | 2007-09-19 | 南京工业大学 | Preparation method of oil-filled insoluble sulphur |
| CN203568846U (en) * | 2013-10-12 | 2014-04-30 | 江苏宏泰橡胶助剂有限公司 | Device for preparing high-quality insoluble sulphur |
| CN208265778U (en) * | 2018-03-19 | 2018-12-21 | 无锡华盛橡胶新材料科技股份有限公司 | A kind of production equipment of oil-filled insoluble sulfur |
| CN109126602A (en) * | 2018-09-18 | 2019-01-04 | 北京燕山粉研精机有限公司 | Powder liquid continuous mixer and continuous metering mixture manufacturing line |
| CN210131550U (en) * | 2019-05-22 | 2020-03-10 | 宜昌阿波罗肥业有限公司 | Compound fertilizer material adjusting device |
| CN211636311U (en) * | 2019-08-17 | 2020-10-09 | 青岛凯立德生物科技有限公司 | Fat powder blending device convenient to clean |
| CN113522074A (en) * | 2020-04-15 | 2021-10-22 | 中国石油化工股份有限公司 | Powder-liquid mixing equipment |
| CN111547684A (en) * | 2020-05-13 | 2020-08-18 | 山东润初企业管理咨询有限责任公司 | Production method of insoluble sulfur and insoluble sulfur |
| CN212632322U (en) * | 2020-05-18 | 2021-03-02 | 太阳树(莆田)生物医药有限公司 | A blendor for plant draws |
| KR20220001936A (en) * | 2020-06-30 | 2022-01-06 | 주식회사 엔티시스템 | Manufacturing method of insoluble sulfur |
| CN214635879U (en) * | 2020-12-28 | 2021-11-09 | 中原环保郑州污泥新材料科技有限公司 | Mixing arrangement is used in flocculating agent production |
Non-Patent Citations (1)
| Title |
|---|
| 梁朝林编著.《高硫原油加工》.中国石化出版社,2001,第137页. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114100473A (en) | 2022-03-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US20020033131A1 (en) | Coated polymeric particles having improved anti-block characteristics, method of making such particles, and apparatus therefor | |
| CN114100473B (en) | Continuous oil filling method and oil filling mixing device for insoluble sulfur | |
| US5368385A (en) | Continuous solution method and apparatus | |
| CN109277026A (en) | A kind of fine agitating device of coating | |
| EP2207615A2 (en) | Control of particle formation | |
| CN108097162A (en) | It is granulated using melting drip-type come the equipment and its processing method of processing rubber auxiliary agent | |
| CA1139608A (en) | Process for producing a gasified fusible sugar composition | |
| EP0216182B1 (en) | Apparatus and process for producing gel beads of microbial cells or enzyme | |
| CN104884154A (en) | Method for granulating meltable materials | |
| CN112742486B (en) | Oil column catalyst forming device and forming method | |
| CN113522074A (en) | Powder-liquid mixing equipment | |
| CN213965191U (en) | Spray drying device | |
| CN101844049A (en) | Multidirectional three-level mixing device and method thereof | |
| CN111457677B (en) | Online drying and mixing system and method for superfine powder | |
| CN206262383U (en) | Material mixing device | |
| CN210139525U (en) | Production line for wet-method refining of powdered rubber | |
| EP3801883A1 (en) | Apparatus and process for continuous adsorption | |
| CN220235998U (en) | Fodder spraying system | |
| CN101862616A (en) | Distributed two-stage mixing device and method thereof | |
| CN219278597U (en) | Discharging device for ammonium bifluoride drying | |
| CN204619406U (en) | Hydronic centrifugal spray dryer shower nozzle | |
| JPH09227838A (en) | Apparatus for continuously forming stock paste by dissolution | |
| CN205182547U (en) | Poor controlling means of PET bottle piece granule secondary color | |
| CN218053419U (en) | Plastic particle mixing and stirring synthesizer | |
| CN201586501U (en) | Double stirring type two-stage mixing device with premixing tower |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |