CN116651020A - Separation device for dimethyl disulfide production and manufacturing and application method thereof - Google Patents
Separation device for dimethyl disulfide production and manufacturing and application method thereof Download PDFInfo
- Publication number
- CN116651020A CN116651020A CN202310949208.7A CN202310949208A CN116651020A CN 116651020 A CN116651020 A CN 116651020A CN 202310949208 A CN202310949208 A CN 202310949208A CN 116651020 A CN116651020 A CN 116651020A
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- dimethyl
- liquid
- pipe
- bin
- dimethyl disulfide
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- WQOXQRCZOLPYPM-UHFFFAOYSA-N dimethyl disulfide Chemical compound CSSC WQOXQRCZOLPYPM-UHFFFAOYSA-N 0.000 title claims abstract description 244
- 238000000926 separation method Methods 0.000 title claims abstract description 35
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000007788 liquid Substances 0.000 claims abstract description 167
- YWHLKYXPLRWGSE-UHFFFAOYSA-N Dimethyl trisulfide Chemical compound CSSSC YWHLKYXPLRWGSE-UHFFFAOYSA-N 0.000 claims abstract description 107
- NPNIZCVKXVRCHF-UHFFFAOYSA-N dihydrocarbyl tetrasulfide Natural products CSSSSC NPNIZCVKXVRCHF-UHFFFAOYSA-N 0.000 claims abstract description 32
- UJRYDUDEJGXDNA-UHFFFAOYSA-N quinoline-4-sulfonic acid Chemical compound C1=CC=C2C(S(=O)(=O)O)=CC=NC2=C1 UJRYDUDEJGXDNA-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000001704 evaporation Methods 0.000 claims abstract description 23
- 230000008020 evaporation Effects 0.000 claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims description 23
- 230000002572 peristaltic effect Effects 0.000 claims description 20
- 238000007789 sealing Methods 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 16
- 238000009835 boiling Methods 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 9
- 238000005192 partition Methods 0.000 claims description 6
- 238000009833 condensation Methods 0.000 claims description 4
- 230000005494 condensation Effects 0.000 claims description 4
- 230000009471 action Effects 0.000 claims description 3
- 230000005540 biological transmission Effects 0.000 claims description 3
- 229910010293 ceramic material Inorganic materials 0.000 claims description 3
- 238000001802 infusion Methods 0.000 claims description 2
- QMMFVYPAHWMCMS-UHFFFAOYSA-N Dimethyl sulfide Chemical compound CSC QMMFVYPAHWMCMS-UHFFFAOYSA-N 0.000 claims 38
- 238000011176 pooling Methods 0.000 claims 2
- 238000000746 purification Methods 0.000 abstract description 4
- LSDPWZHWYPCBBB-UHFFFAOYSA-N Methanethiol Chemical compound SC LSDPWZHWYPCBBB-UHFFFAOYSA-N 0.000 description 10
- 230000000694 effects Effects 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 125000004122 cyclic group Chemical group 0.000 description 4
- 230000005611 electricity Effects 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 3
- 230000033001 locomotion Effects 0.000 description 3
- 238000004073 vulcanization Methods 0.000 description 3
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 238000005486 sulfidation Methods 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004517 catalytic hydrocracking Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005906 dihydroxylation reaction Methods 0.000 description 1
- VAYGXNSJCAHWJZ-UHFFFAOYSA-N dimethyl sulfate Chemical compound COS(=O)(=O)OC VAYGXNSJCAHWJZ-UHFFFAOYSA-N 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention discloses a separation device for producing and manufacturing dimethyl disulfide and a use method thereof, relating to the technical field of dimethyl disulfide production, and comprising a chassis, an evaporation tank, a centrifugal bin and a controller; a top plate is arranged above the underframe, four supporting rods are fixedly connected to corners of the bottom surface of the top plate, the bottom ends of the supporting rods are fixedly connected to the top surface of the underframe, transverse plates are fixedly connected between the four supporting rods, and the transverse plates are positioned between the underframe and the top plate; the evaporation box is fixedly arranged on the upper surface of the top plate and is used for evaporating dimethyl trisulfide in dimethyl disulfide liquid. According to the invention, through a centrifugal separation mode, doped dimethyl trisulfide and dimethyl tetrasulfide can be separated from dimethyl disulfide liquid in a non-stop state, so that the purity of dimethyl disulfide is ensured, the separation efficiency is high, and the purification process of dimethyl disulfide can be simplified.
Description
Technical Field
The invention relates to the technical field of dimethyl disulfide production, in particular to a separation device for dimethyl disulfide production and manufacturing and a use method thereof.
Background
Dimethyl disulfide is an important organic chemical product, and can be widely used for preparing intermediates of pesticide; in the petroleum industry, can be used as an anti-corrosion and anti-coking agent of an ethane cracking furnace, a vulcanizing machine in gasoline hydrogenation catalysis and an inhibitor for hydrocracking in benzene ring dehydroxylation reaction; in the rubber industry, can be used as solvents, regenerators, softeners, plasticizers, etc.; in addition, dimethyl disulfide is also useful as an additive for fuels and lubricating oils.
In the technology of industrially producing dimethyl disulfide, there are four production methods of dimethyl disulfide: dimethyl sulfate process, methyl mercaptan oxidation process, methanol sulfidation process and methyl mercaptan sulfidation process. At present, in the related reports and patents of the methyl mercaptan vulcanization method for producing dimethyl disulfide, the following two production methods are mainly available:
the method has the advantages that the sulfur and the methyl mercaptan serving as raw materials react in a vulcanization reactor to generate dimethyl disulfide, and the reacted materials enter a rectifying tower for refining and separation.
The other is to produce dimethyl disulfide through cyclic vulcanization reaction, which is the main stream method for industrial production of dimethyl disulfide at present, namely CN103864650A discloses a continuous production method of dimethyl disulfide, which is characterized in that raw material sulfur is melted and then is sent into a dimethyl trisulfide reactor through a feed pump to react with the cyclic dimethyl disulfide to generate dimethyl trisulfide, the dimethyl trisulfide and methyl mercaptan enter the dimethyl disulfide reactor to react to generate dimethyl disulfide, a crude dimethyl disulfide product enters a separation tank to separate most of hydrogen sulfide, a liquid phase product enters a rectifying tower, the dimethyl disulfide product is recovered through condensation at the top of the tower, the hydrogen sulfide is discharged as noncondensable gas, and the dimethyl disulfide and the dimethyl trisulfide in the tower reactor are returned to the dimethyl trisulfide reactor again to continue the cyclic reaction. In the production method, the separation device used comprises a separation tank, a rectifying tower, an overhead condenser and a tower kettle reactor.
Based on the technical scheme of the patent (i.e. CN103864650A discloses a method for continuously producing dimethyl disulfide) and combining with a separation device in the prior art, in the current production practice process, the dimethyl disulfide and dimethyl trisulfide in a tower reactor are returned to the dimethyl trisulfide reactor again for continuous cyclic reaction, and finally reacted materials enter a single rectifying tower for refining separation, so that the concentration of the dimethyl trisulfide contained in the dimethyl disulfide solution circulated in the tower is higher, and a small amount of dimethyl tetrasulfide is also produced. In order to separate dimethyl trisulfide and dimethyl tetrasulfide from dimethyl disulfide and improve the purity of the dimethyl disulfide, a separation device for producing and manufacturing dimethyl disulfide and a use method thereof are provided.
Disclosure of Invention
The invention aims to make up the defects of the prior art, and provides a separation device for producing and manufacturing dimethyl disulfide and a use method thereof, which can separate doped dimethyl trisulfide and dimethyl tetrasulfide from dimethyl disulfide liquid under the condition of no shutdown, ensure the purity of the dimethyl disulfide, have high separation efficiency and can simplify the purification procedure of the dimethyl disulfide.
The invention provides the following technical scheme for solving the technical problems: a separation device for producing and manufacturing dimethyl disulfide comprises a bottom frame, an evaporation tank, a centrifugal bin and a controller;
a top plate is arranged above the underframe, four supporting rods are fixedly connected to corners of the bottom surface of the top plate, the bottom ends of the supporting rods are fixedly connected to the top surface of the underframe, transverse plates are fixedly connected between the four supporting rods, and the transverse plates are positioned between the underframe and the top plate;
the evaporation box is fixedly arranged on the upper surface of the top plate and is used for evaporating dimethyl trisulfide in dimethyl disulfide liquid.
The centrifugal bin is hollow sphere, and the centrifugal bin sets up between chassis and diaphragm, the fixed intercommunication in top in centrifugal bin has the feed liquor pipe, the surface of feed liquor pipe is rotated through the bearing and is connected in the middle part of diaphragm, and the top of feed liquor pipe extends to the top of diaphragm, the inside cover of feed liquor pipe is equipped with the drain pipe, the top fixed connection of feed liquor pipe is in the surface of drain pipe, and the top and the drain pipe sealing connection of feed liquor pipe.
The top of drain pipe runs through to the top of roof and is linked together with the evaporation case, the bottom of drain pipe extends to the inside of centrifugal storehouse and with the interior bottom wall fixed connection in centrifugal storehouse.
The inner wall of centrifugal storehouse and the surface of drain pipe between fixedly connected with a plurality of baffles, a plurality of the baffle is cut apart the inner chamber of centrifugal storehouse into a plurality of centrifugal chambeies R, can cut apart the inside of centrifugal storehouse into a plurality of independent spaces, when centrifugal storehouse and its inside liquid rotate in the lump, can reduce the liquid in centrifugal storehouse and produce the condition of vortex, guarantees centrifugal effect, a plurality of drain holes have been seted up to the surface of drain pipe bottom.
The outer surface of feed liquor pipe rotates and cup joints first intercommunication ware, and first intercommunication ware passes through sealing washer and the surface sealing connection of feed liquor pipe, the feed liquor hole that is linked together with the inner chamber of first intercommunication ware is seted up to the surface of feed liquor pipe, the surface fixed intercommunication of first intercommunication ware has the transfer line, the surface of first intercommunication ware passes through connecting rod and roof bottom surface fixed connection.
The bottom fixedly connected with collecting pipe in centrifugal storehouse, the surface of collecting pipe passes through the bearing and rotates the middle part of being connected in the chassis, and the bottom of collecting pipe extends to the below of chassis, the bottom surface fixedly connected with motor of chassis, the output of motor passes through belt pulley and belt and collecting pipe transmission and is connected.
The surface rotation of collecting pipe has cup jointed the second intercommunication ware, and the second intercommunication ware passes through sealing washer and the surface sealing connection of collecting pipe, the surface of second intercommunication ware passes through the bottom surface fixed connection of connecting rod and chassis, the liquid guide hole that is linked together with the inner chamber of second intercommunication ware is seted up to the surface of collecting pipe, the surface fixed intercommunication of second intercommunication ware has the catheter, the one end fixed intercommunication that the second intercommunication ware was kept away from to the catheter has the peristaltic pump, the middle section of catheter is provided with pressure sensor, and pressure sensor sets up between peristaltic pump and second intercommunication ware, pressure sensor is connected with the signal end electricity of controller, the control end and the peristaltic pump electricity of controller are connected.
The outer surface of the centrifugal bin is hermetically sleeved with a first annular collecting bin, and the outer surface of the first annular collecting bin is hermetically sleeved with a second annular collecting bin.
The centrifugal bin is characterized in that a plurality of first material drawing holes are formed in the outer surface of the centrifugal bin, and the centrifugal cavity R is communicated with the inner cavity of the first annular collecting bin through the first material drawing holes.
The outer surface of the first annular collecting bin is provided with a plurality of second material drawing holes, and the inner cavity of the first annular collecting bin is communicated with the inner cavity of the second annular collecting bin through the second material drawing holes.
The outer surface fixed intercommunication of storehouse is collected to the second annular has a plurality of arced tube, every the bottom of arced tube all with the fixed intercommunication of collecting pipe.
The evaporation box comprises a constant temperature heating box fixedly connected to the top surface of the top plate, a liquid discharge pipe is fixedly communicated with the middle of the constant temperature heating box, and an exhaust pipe is fixedly communicated with the top of the constant temperature heating box.
The annular filter element is fixedly arranged between the inner wall of the liquid inlet pipe and the outer surface of the liquid outlet pipe, a plurality of guide plates are fixedly arranged between the inner wall of the liquid inlet pipe and the outer surface of the liquid outlet pipe, the guide plates divide the cavity inside the liquid inlet pipe into a plurality of guide cavities T, and the number of the guide plates is equal to that of the partition plates.
The inner wall of the first annular collecting bin is fixedly provided with a first annular buffer piece, the inner wall of the second annular collecting bin is fixedly provided with a second annular buffer piece, and the first annular buffer piece and the second annular buffer piece are made of porous ceramic materials.
The use method of the separation device for producing and manufacturing dimethyl disulfide comprises the following steps:
s1, delivering dimethyl disulfide liquid into the first communicating vessel through a liquid delivery pipe by utilizing a liquid pump, enabling the dimethyl disulfide liquid to flow into an inner cavity of the liquid delivery pipe through a liquid inlet hole and flow into the centrifugal bin, then flowing into a liquid outlet pipe through a liquid outlet hole, then flowing into an evaporation tank from the top end of the liquid outlet pipe, and finally flowing out through a liquid discharge pipe to realize the circulation of the dimethyl disulfide liquid in the device;
s2, in the process of circulating the dimethyl disulfide liquid in the device, a motor is started to rotate at a constant speed, the motor drives a collecting pipe, a centrifugal bin and a liquid inlet pipe to rotate together, at the moment, a first annular collecting bin, a second annular collecting bin, an arc-shaped pipe and a liquid outlet pipe also synchronously rotate, the dimethyl disulfide liquid synchronously rotates in the liquid inlet pipe, the centrifugal bin, the first annular collecting bin and the arc-shaped pipe, when the dimethyl disulfide liquid flows through a centrifugal cavity, because the centrifugal force generated by rotation is generated, and because the density value of the dimethyl disulfide is less than the density value of the dimethyl trisulfide less than the density value of the dimethyl tetrasulfide, the dimethyl trisulfide and the dimethyl tetrasulfide doped in the dimethyl disulfide liquid can be gradually gathered towards the edge of an inner cavity of the centrifugal bin, and then enter the inner cavity of the first annular collecting bin through a first drawing hole to be accumulated for the first time, collecting the dimethyl trisulfide and the dimethyl tetrasulfide doped in the dimethyl disulfide liquid into the inner cavity of the second annular collecting bin through the second material drawing hole, finally collecting the dimethyl trisulfide and the dimethyl tetrasulfide in the dimethyl disulfide liquid through the arc-shaped pipe, gradually increasing the concentration of the dimethyl trisulfide and the dimethyl tetrasulfide accumulated in the first annular collecting bin and the second annular collecting bin along with the gradual increase of the content of the dimethyl trisulfide and the dimethyl tetrasulfide in the first annular collecting bin and the second annular collecting bin, gradually increasing the liquid pressure values in the first annular collecting bin, the second annular collecting bin, the arc-shaped pipe and the collecting pipe under the action of centrifugal force, gradually increasing the pressure values detected by the pressure sensor, judging the collecting condition of the dimethyl trisulfide and the dimethyl tetrasulfide in the first annular collecting bin and the second annular collecting bin according to the pressure value of the pressure sensor, the working state of the peristaltic pump is controlled according to the collection condition of the dimethyl trisulfide and the dimethyl tetrasulfide, namely, the pressure value of the pressure sensor is fed back to the controller, when the pressure value of the pressure sensor reaches the threshold value set by the controller, the peristaltic pump is controlled to be started by the controller, the dimethyl trisulfide and the dimethyl tetrasulfide in the first annular collecting bin, the second annular collecting bin, the arc-shaped pipe and the collecting pipe are discharged, the dimethyl trisulfide and the dimethyl tetrasulfide doped in the dimethyl disulfide liquid can be accurately separated, and when the pressure value detected by the pressure sensor is restored to a set value interval, the peristaltic pump stops working;
s3, after the dimethyl disulfide liquid is centrifugally separated in the centrifugal bin, the dimethyl disulfide liquid flows into the constant temperature heating box through the liquid outlet hole and the liquid outlet pipe, the constant temperature of the constant temperature heating box is set to be between 45 ℃ and 50 ℃, and because the boiling point of dimethyl disulfide is 109 ℃, the boiling point of dimethyl trisulfide is 41 ℃, and the boiling point of dimethyl tetrasulfide is greater than 243 ℃, the dimethyl disulfide liquid is evaporated when the dimethyl trisulfide doped in the dimethyl disulfide liquid flows through the inside of the constant temperature heating box, the evaporated dimethyl trisulfide steam is discharged to a condenser through an exhaust pipe for condensation collection, the purity of the dimethyl disulfide liquid in the constant temperature heating box can be further improved, and finally, the obtained high-purity dimethyl disulfide is discharged and collected through the liquid outlet pipe.
Compared with the prior art, the separating device for producing and manufacturing the dimethyl disulfide and the using method thereof have the following beneficial effects:
1. according to the invention, through a centrifugal separation mode, doped dimethyl trisulfide and dimethyl tetrasulfide can be separated from dimethyl disulfide liquid in a non-stop state, so that the purity of dimethyl disulfide is ensured, the separation efficiency is high, and the purification process of dimethyl disulfide can be simplified.
2. According to the invention, after doped dimethyl trisulfide and dimethyl tetrasulfide are separated from the dimethyl disulfide liquid in a centrifugal separation mode, a small amount of dimethyl trisulfide remained in the dimethyl disulfide liquid is separated by utilizing an evaporation tank, and the dimethyl trisulfide remained in the dimethyl disulfide liquid can be removed only by heating the dimethyl disulfide liquid to 45-50 ℃, so that the purity of the dimethyl disulfide liquid can be further improved, and compared with the traditional distillation separation method, the method is more energy-saving and environment-friendly.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Drawings
FIG. 1 is a schematic perspective view of a separation device for producing and manufacturing dimethyl disulfide;
FIG. 2 is a cross-sectional view of the separation device for producing dimethyl disulfide from the front view;
FIG. 3 is a schematic perspective view of a centrifugal cartridge, a liquid inlet pipe and a collecting pipe according to the present invention;
FIG. 4 is a detailed view showing the internal structure of the liquid inlet pipe and the first communicating vessel in FIG. 2 according to the present invention;
FIG. 5 is a detailed view of the internal structure of the centrifugal cartridge of FIG. 2 according to the present invention;
FIG. 6 is a detailed view of the structure of the collection tube of FIG. 2 according to the present invention;
FIG. 7 is a schematic cross-sectional view of the centrifugal cartridge, first annular collection cartridge and second annular collection cartridge of the present invention from a bottom view;
FIG. 8 is a schematic cross-sectional view of a liquid inlet pipe according to the present invention.
In the figure:
1. a chassis; 2. a top plate; 3. a support rod; 4. a cross plate;
5. an evaporation tank; 51. a constant temperature heating box; 52. a liquid discharge pipe; 53. an exhaust pipe;
6. a centrifugal bin; 61. a first annular collection bin; 62. a second annular collection bin; 63. a partition plate; 64. a first digging hole; 65. a second digging hole; 66. an arc tube; 67. a first annular buffer; 68. a second annular buffer;
7. a liquid inlet pipe; 71. a first communicator; 72. a liquid inlet hole; 73. an annular filter element; 74. a deflector; 75. an infusion tube;
8. a liquid outlet pipe; 801. a liquid outlet hole;
9. a collection pipe; 91. a second communicating vessel; 92. a liquid guiding hole; 93. a catheter;
10. a peristaltic pump; 11. a pressure sensor; 12. a motor; r, centrifugal cavity; t, a diversion cavity.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Referring to fig. 1 to 8, the present invention provides the following technical solutions: a separation device for producing and manufacturing dimethyl disulfide comprises a bottom frame 1, an evaporation tank 5, a centrifugal bin 6 and a controller.
The top of chassis 1 is equipped with roof 2, and the corner fixedly connected with four branches 3 of roof 2 bottom surface, the equal fixed connection in the top surface of chassis 1 of bottom of every branch 3, fixedly connected with diaphragm 4 between four branches 3, and diaphragm 4 is located between chassis 1 and the roof 2.
The evaporation tank 5 is fixedly arranged on the upper surface of the top plate 2, and the evaporation tank 5 is used for evaporating the dimethyl trisulfide in the dimethyl disulfide liquid.
The centrifugal bin 6 is hollow sphere, and the centrifugal bin 6 sets up between chassis 1 and diaphragm 4, and the fixed intercommunication in top of centrifugal bin 6 has feed liquor pipe 7, and the surface of feed liquor pipe 7 passes through the bearing and rotates the middle part of being connected in diaphragm 4, and the top of feed liquor pipe 7 extends to the top of diaphragm 4, and the inside cover of feed liquor pipe 7 is equipped with drain pipe 8, and the top fixed connection of feed liquor pipe 7 is in the surface of drain pipe 8, and the top of feed liquor pipe 7 and drain pipe 8 sealing connection.
The top of drain pipe 8 runs through to the top of roof 2 and is linked together with evaporating box 5, and the bottom of drain pipe 8 extends to the inside of centrifugal storehouse 6 and is connected with the interior bottom wall fixed of centrifugal storehouse 6.
Fixedly connected with a plurality of baffles 63 between the inner wall of centrifugal storehouse 6 and the surface of drain pipe 8, a plurality of centrifugal chamber R are cut apart into to the inner chamber of centrifugal storehouse 6 to a plurality of baffles 63, can cut apart the inside of centrifugal storehouse 6 into a plurality of independent spaces, and when centrifugal storehouse 6 and its inside liquid were rotatory in the lump, the condition that the liquid that can reduce centrifugal storehouse 6 produced the vortex guaranteed centrifugal effect, a plurality of drain holes 801 have been seted up to the surface of drain pipe 8 bottom.
The outer surface of the liquid inlet pipe 7 is rotatably sleeved with a first communicating vessel 71, the first communicating vessel 71 is in sealing connection with the outer surface of the liquid inlet pipe 7 through a sealing ring, a liquid inlet hole 72 communicated with the inner cavity of the first communicating vessel 71 is formed in the outer surface of the liquid inlet pipe 7, a liquid conveying pipe 75 is fixedly communicated with the outer surface of the first communicating vessel 71, and the outer surface of the first communicating vessel 71 is fixedly connected with the bottom surface of the top plate 2 through a connecting rod.
The bottom fixedly connected with collecting pipe 9 of centrifugal storehouse 6, the surface of collecting pipe 9 passes through the bearing and rotates the middle part of being connected in chassis 1, and the bottom of collecting pipe 9 extends to the below of chassis 1, and the bottom surface fixedly connected with motor 12 of chassis 1, the output of motor 12 passes through belt pulley and belt and collecting pipe 9 transmission is connected.
The surface rotation of collecting pipe 9 has cup jointed second intercommunication ware 91, and second intercommunication ware 91 passes through sealing washer and the surface sealing connection of collecting pipe 9, the surface of second intercommunication ware 91 passes through the bottom surface fixed connection of connecting rod and chassis 1, the drain hole 92 that is linked together with the inner chamber of second intercommunication ware 91 is seted up to the surface of collecting pipe 9, the surface fixed intercommunication of second intercommunication ware 91 has catheter 93, the one end fixed intercommunication that second intercommunication ware 91 was kept away from to catheter 93 has peristaltic pump 10, catheter 93's middle section is provided with pressure sensor 11, and pressure sensor 11 sets up between peristaltic pump 10 and second intercommunication ware 91, pressure sensor 11 is connected with the signal end electricity of controller, the control end and the peristaltic pump 10 electricity of controller are connected.
The outer surface of the centrifugal bin 6 is hermetically sleeved with a first annular collecting bin 61, and the outer surface of the first annular collecting bin 61 is hermetically sleeved with a second annular collecting bin 62.
The outer surface of the centrifugal bin 6 is provided with a plurality of first material drawing holes 64, and the centrifugal cavity R is communicated with the inner cavity of the first annular collecting bin 61 through the first material drawing holes 64.
The outer surface of the first annular collecting bin 61 is provided with a plurality of second material drawing holes 65, and the inner cavity of the first annular collecting bin 61 is communicated with the inner cavity of the second annular collecting bin 62 through the second material drawing holes 65.
The outer surface of the second annular collecting bin 62 is fixedly communicated with a plurality of arc-shaped pipes 66, and the bottom end of each arc-shaped pipe 66 is fixedly communicated with the collecting pipe 9.
The evaporation tank 5 comprises a constant temperature heating tank 51 fixedly connected to the top surface of the top plate 2, a liquid discharge pipe 52 is fixedly communicated with the middle of the constant temperature heating tank 51, and an exhaust pipe 53 is fixedly communicated with the top of the constant temperature heating tank 51.
The using method and the working principle of the separating device for producing and manufacturing the dimethyl disulfide are as follows:
s1, delivering dimethyl disulfide liquid into the first connector 71 through a liquid delivery pipe 75 by using a liquid pump, enabling the dimethyl disulfide liquid to flow into the inner cavity of the liquid inlet pipe 7 through a liquid inlet hole 72 and flow into the centrifugal bin 6, then flowing into the liquid outlet pipe 8 through a liquid outlet hole 801, then flowing into the evaporation tank 5 from the top end of the liquid outlet pipe 8, and finally flowing out through a liquid discharge pipe 52, so as to realize the circulation of the dimethyl disulfide liquid in the device;
s2, in the process of circulating the dimethyl disulfide liquid in the device, the motor 12 is started to rotate at a constant speed, the motor 12 drives the collecting pipe 9, the centrifugal bin 6 and the liquid inlet pipe 7 to rotate together, at the moment, the first annular collecting bin 61, the second annular collecting bin 62, the arc-shaped pipe 66 and the liquid outlet pipe 8 also synchronously rotate, the dimethyl disulfide liquid synchronously rotates in the liquid inlet pipe 7, the centrifugal bin 6, the first annular collecting bin 61 and the arc-shaped pipe 66, when the dimethyl disulfide liquid flows through the centrifugal cavity R, because of centrifugal force generated by rotation, and because the density value of dimethyl disulfide is less than that of dimethyl trisulfide is less than that of dimethyl tetrasulfide, the dimethyl trisulfide and the dimethyl tetrasulfide doped in the dimethyl disulfide liquid can be gradually gathered towards the edge of the inner cavity of the centrifugal bin 6, then enters the inner cavity of the first annular collecting bin 61 through the first material drawing hole 64 for primary accumulation, then is collected into the inner cavity of the second annular collecting bin 62 through the second material drawing hole 65, finally is collected into the inner cavity of the collecting tube 9 through the arc tube 66 to separate dimethyl trisulfide and dimethyl tetrasulfide doped in the dimethyl disulfide liquid, as the content of the dimethyl trisulfide and the dimethyl tetrasulfide accumulated in the inner parts of the first annular collecting bin 61 and the second annular collecting bin 62 is gradually increased, the liquid density in the first annular collecting bin 61 and the second annular collecting bin 62 is also gradually increased under the action of centrifugal force, the liquid pressure values in the first annular collecting bin 61, the second annular collecting bin 62, the arc tube 66 and the collecting tube 9 are also gradually increased, the pressure value detected by the pressure sensor 11 is also increased, the collecting conditions of the dimethyl trisulfide and the dimethyl tetrasulfide in the first annular collecting bin 61 and the second annular collecting bin 62 can be judged according to the pressure value of the pressure sensor 11, so that the working state of the peristaltic pump 10 is controlled according to the collecting conditions of the dimethyl trisulfide and the dimethyl tetrasulfide, namely, the pressure value of the pressure sensor 11 is fed back to the controller, when the pressure value of the pressure sensor 11 reaches the threshold value set by the controller, the peristaltic pump 10 is controlled to be started by the controller, the dimethyl trisulfide and the dimethyl tetrasulfide in the first annular collecting bin 61, the second annular collecting bin 62, the arc-shaped pipe 66 and the collecting pipe 9 are discharged, and the dimethyl trisulfide and the dimethyl tetrasulfide doped in the dimethyl disulfide liquid can be accurately separated, when the pressure value detected by the pressure sensor 11 is recovered to the set value interval, the peristaltic pump 10 stops working, and when the pressure value of the pressure sensor 11 reaches the threshold value set by the controller, the peristaltic pump 10 is started again;
s3, after the dimethyl disulfide liquid is centrifugally separated in the centrifugal bin 6, the dimethyl disulfide liquid flows into the constant temperature heating box 51 through the liquid outlet hole 801 and the liquid outlet pipe 8, the constant temperature of the constant temperature heating box 51 is set to be between 45 ℃ and 50 ℃, and because the boiling point of the dimethyl disulfide is 109 ℃, the boiling point of the dimethyl trisulfide is 41 ℃, and the boiling point of the dimethyl tetrasulfide is higher than 243 ℃, the dimethyl disulfide liquid is evaporated when flowing through the inside of the constant temperature heating box 51, the dimethyl trisulfide doped in the dimethyl disulfide liquid is evaporated at 45 ℃, the evaporated dimethyl trisulfide steam is discharged to a condenser through the exhaust pipe 53 for condensation collection, the purity of the dimethyl disulfide liquid in the constant temperature heating box 51 can be further improved, and finally, the obtained high-purity dimethyl disulfide is discharged and collected through the liquid outlet pipe 52.
In summary, the device can separate doped dimethyl trisulfide and dimethyl tetrasulfide from dimethyl disulfide liquid in a centrifugal separation mode without stopping, ensures the purity of dimethyl disulfide, has high separation efficiency, and can simplify the purification process of dimethyl disulfide.
Further, an annular filter element 73 is fixedly arranged between the inner wall of the liquid inlet pipe 7 and the outer surface of the liquid outlet pipe 8, a plurality of guide plates 74 are fixedly arranged between the inner wall of the liquid inlet pipe 7 and the outer surface of the liquid outlet pipe 8, the plurality of guide plates 74 divide the cavity inside the liquid inlet pipe 7 into a plurality of guide cavities T, and the number of the guide plates 74 is equal to that of the partition plates 63.
Through above-mentioned scheme, before dimethyl disulfide liquid gets into centrifugal storehouse 6, because motor 12 drives collecting pipe 9, centrifugal storehouse 6 and feed liquor pipe 7 and carries out high-speed rotation, dimethyl disulfide liquid very easily takes place the vortex when getting into feed liquor pipe 7 and centrifugal storehouse 6, and influence the centrifugal effect to dimethyl disulfide liquid, through annular filter core 73 and a plurality of guide plates 74 that set up, can slow down the vortex motion that dimethyl disulfide liquid took place in the inside of feed liquor pipe 7, realize dimethyl disulfide liquid and feed liquor pipe 7 and centrifugal storehouse 6 synchronous rotatory state fast, guarantee centrifugal effect.
Further, the inner wall of the first annular collecting bin 61 is fixedly provided with a first annular buffer member 67, the inner wall of the second annular collecting bin 62 is fixedly provided with a second annular buffer member 68, and the first annular buffer member 67 and the second annular buffer member 68 are both made of porous ceramic materials.
The dimethyl trithio and the dimethyl tetrathiofide after centrifugal separation are collected into the inner cavity of the first annular collecting bin 61 and the inner cavity of the second annular collecting bin 62, and then mixed liquid of the dimethyl trithio and the dimethyl tetrathiofide is discharged by starting the peristaltic pump 10, in the discharging process, vortex is easily generated in the inner cavity of the first annular collecting bin 61 and the inner cavity of the second annular collecting bin 62, and vortex movement generated in the first annular collecting bin 61 and the second annular collecting bin 62 can be slowed down through the first annular buffer piece 67 and the second annular buffer piece 68, so that irregular and disordered movement of the liquid is avoided, the separation effect between the dimethyl trithio, the dimethyl tetrathiofide and the dimethyl disulfide is further ensured, and the purity of the dimethyl disulfide is improved.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. The utility model provides a dimethyl disulfide production separator for manufacturing, includes chassis (1), evaporating box (5), centrifugal storehouse (6) and controller, its characterized in that: a top plate (2) is arranged above the underframe (1), four supporting rods (3) are fixedly connected to corners of the bottom surface of the top plate (2), the bottom ends of the supporting rods (3) are fixedly connected to the top surface of the underframe (1), a transverse plate (4) is fixedly connected between the four supporting rods (3), and the transverse plate (4) is positioned between the underframe (1) and the top plate (2);
the evaporation bin (5) is fixedly arranged on the upper surface of the top plate (2), the centrifugal bin (6) is a hollow sphere, the centrifugal bin (6) is arranged between the underframe (1) and the transverse plate (4), the top of the centrifugal bin (6) is fixedly communicated with the liquid inlet pipe (7), the outer surface of the liquid inlet pipe (7) is rotationally connected to the middle part of the transverse plate (4) through a bearing, the top of the liquid inlet pipe (7) extends to the upper part of the transverse plate (4), a liquid outlet pipe (8) is sleeved in the liquid inlet pipe (7), the top of the liquid inlet pipe (7) is fixedly connected to the outer surface of the liquid outlet pipe (8), the top of the liquid outlet pipe (7) is in sealing connection with the liquid outlet pipe (8), the top of the liquid outlet pipe (8) penetrates to the upper part of the top plate (2) and is communicated with the evaporation bin (5), and the bottom of the liquid outlet pipe (8) extends to the inner bottom wall of the centrifugal bin (6) and is fixedly connected with the inner bottom wall of the centrifugal bin (6);
a plurality of partition boards (63) are fixedly connected between the inner wall of the centrifugal bin (6) and the outer surface of the liquid outlet pipe (8), the partition boards (63) divide the inner cavity of the centrifugal bin (6) into a plurality of centrifugal cavities (R), and a plurality of liquid outlet holes (801) are formed in the outer surface of the bottom end of the liquid outlet pipe (8);
the outer surface of the liquid inlet pipe (7) is rotationally sleeved with a first communicating vessel (71), the first communicating vessel (71) is in sealing connection with the outer surface of the liquid inlet pipe (7) through a sealing ring, a liquid inlet hole (72) communicated with the inner cavity of the first communicating vessel (71) is formed in the outer surface of the liquid inlet pipe (7), an infusion tube (75) is fixedly communicated with the outer surface of the first communicating vessel (71), and the outer surface of the first communicating vessel (71) is fixedly connected with the bottom surface of the top plate (2) through a connecting rod;
the bottom of the centrifugal bin (6) is fixedly connected with a collecting pipe (9), the outer surface of the collecting pipe (9) is rotationally connected to the middle part of the underframe (1) through a bearing, the bottom end of the collecting pipe (9) extends to the lower part of the underframe (1), the outer surface of the collecting pipe (9) is rotationally sleeved with a second communicating vessel (91), the second communicating vessel (91) is in sealing connection with the outer surface of the collecting pipe (9) through a sealing ring, the outer surface of the second communicating vessel (91) is fixedly connected with the bottom surface of the underframe (1) through a connecting rod, the outer surface of the collecting pipe (9) is provided with a liquid guide hole (92) communicated with the inner cavity of the second communicating vessel (91), the outer surface of the second communicating vessel (91) is fixedly communicated with a liquid guide pipe (93), one end of the liquid guide pipe (93) far away from the second communicating vessel (91) is fixedly communicated with a peristaltic pump (10), the middle section of the liquid guide pipe (93) is provided with a pressure sensor (11), the pressure sensor (11) is arranged between the peristaltic pump (10) and the second communicating vessel (91), the outer surface of the pressure sensor (11) is fixedly connected with the control end of the peristaltic pump (11) through a signal controller;
the centrifugal bin is characterized in that a first annular collecting bin (61) is sleeved on the outer surface of the centrifugal bin (6) in a sealing manner, a second annular collecting bin (62) is sleeved on the outer surface of the first annular collecting bin (61) in a sealing manner, a plurality of first material drawing holes (64) are formed in the outer surface of the centrifugal bin (6), a plurality of second material drawing holes (65) are formed in the outer surface of the first annular collecting bin (61), a plurality of arc-shaped pipes (66) are fixedly communicated with the outer surface of the second annular collecting bin (62), and the bottom ends of the arc-shaped pipes (66) are fixedly communicated with the collecting pipe (9).
2. The separation device for producing and manufacturing dimethyl disulfide according to claim 1, wherein: the evaporation box (5) comprises a constant temperature heating box (51) fixedly connected to the top surface of the top plate (2), a liquid discharge pipe (52) is fixedly communicated with the middle part of the constant temperature heating box (51), and an exhaust pipe (53) is fixedly communicated with the top of the constant temperature heating box (51).
3. The separation device for producing and manufacturing dimethyl disulfide according to claim 1, wherein: an annular filter element (73) is fixedly arranged between the inner wall of the liquid inlet pipe (7) and the outer surface of the liquid outlet pipe (8), a plurality of guide plates (74) are fixedly arranged between the inner wall of the liquid inlet pipe (7) and the outer surface of the liquid outlet pipe (8), the guide plates (74) divide the cavity inside the liquid inlet pipe (7) into a plurality of guide cavities (T), and the number of the guide plates (74) is equal to that of the partition plates (63).
4. The separation device for producing and manufacturing dimethyl disulfide according to claim 1, wherein: the inner wall of the first annular collecting bin (61) is fixedly provided with a first annular buffer piece (67), and the inner wall of the second annular collecting bin (62) is fixedly provided with a second annular buffer piece (68).
5. The separation device for producing and manufacturing dimethyl disulfide according to claim 4, wherein: the first annular buffer (67) and the second annular buffer (68) are both made of porous ceramic materials.
6. The separation device for producing and manufacturing dimethyl disulfide according to claim 1, wherein: the bottom surface fixedly connected with motor (12) of chassis (1), the output of motor (12) is connected with collecting pipe (9) transmission through belt pulley and belt.
7. The separation device for producing dimethyl disulfide according to any one of claims 1 to 6, wherein the separation device for producing dimethyl disulfide is used as follows:
s1, delivering dimethyl disulfide liquid into the first connector (71) through a liquid delivery pipe (75) by using a liquid pump, enabling the dimethyl disulfide liquid to flow into the inner cavity of the liquid delivery pipe (7) through a liquid inlet hole (72), flow into the centrifugal bin (6), flow into the liquid outlet pipe (8) through a liquid outlet hole (801), flow into the evaporation tank (5) from the top end of the liquid outlet pipe (8), and flow out through a liquid outlet pipe (52) to realize the circulation of the dimethyl disulfide liquid in the device;
s2, in the process of circulating the dimethyl disulfide liquid in the device, simultaneously starting a motor (12) to enable the dimethyl disulfide liquid to rotate at a constant speed, wherein the motor (12) drives a collecting pipe (9), a centrifugal bin (6) and a liquid inlet pipe (7) to rotate together, at the moment, a first annular collecting bin (61), a second annular collecting bin (62), an arc-shaped pipe (66) and a liquid outlet pipe (8) also synchronously rotate, the dimethyl disulfide liquid synchronously rotates in the liquid inlet pipe (7), the centrifugal bin (6), the first annular collecting bin (61) and the arc-shaped pipe (66), when the dimethyl disulfide liquid flows through a centrifugal cavity (R), because the density value of the dimethyl disulfide is smaller than that of the dimethyl sulfide, the dimethyl sulfide and the dimethyl sulfide doped in the dimethyl disulfide liquid are gradually gathered towards the edge of an inner cavity of the centrifugal bin (6), then enters the inner cavity of the first annular collecting bin (61) through a first material drawing hole (64) to be accumulated, the dimethyl sulfide and the dimethyl sulfide doped in the inner cavity of the first annular collecting bin (62) are gradually gathered into the inner cavity of the first annular collecting bin (62) through the second annular collecting bin (62) and the dimethyl sulfide gradually gathered in the inner cavity (62) is gradually separated from the dimethyl sulfide and the dimethyl sulfide (7) through the annular collecting bin and the second annular collecting bin (62) and the dimethyl sulfide) through the second annular collecting bin and the dimethyl sulfide gradually increased with the dimethyl sulfide (62) and the dimethyl sulfide, the liquid density in the first annular collecting bin (61) and the second annular collecting bin (62) is gradually increased, the liquid pressure values in the first annular collecting bin (61), the second annular collecting bin (62), the arc-shaped pipe (66) and the collecting pipe (9) are also gradually increased under the action of centrifugal force, the pressure values detected by the pressure sensor (11) are also gradually increased, namely, the pooling conditions of the dimethyl trisulfide and the dimethyl tetrasulfide in the first annular collecting bin (61) and the second annular collecting bin (62) can be judged according to the pressure values of the pressure sensor (11), so that the working state of the peristaltic pump (10) is controlled according to the pooling conditions of the dimethyl trisulfide and the dimethyl tetrasulfide, namely, the pressure values of the pressure sensor (11) are fed back to the controller, when the pressure values of the pressure sensor (11) reach the threshold value set by the controller, the peristaltic pump (10) is controlled to be started, the dimethyl trisulfide and the dimethyl tetrasulfide in the collecting bin (61), the second annular collecting bin (66) and the dimethyl tetrasulfide in the collecting pipe (9) are discharged, and the dimethyl trisulfide in the pressure region can be accurately separated, and the dimethyl trisulfide in the pressure region can be recovered to the set value when the dimethyl trisulfide is detected;
s3, after the dimethyl disulfide liquid is centrifugally separated in the centrifugal bin (6), the dimethyl disulfide liquid flows into the constant temperature heating box (51) through the liquid outlet hole (801) and the liquid outlet pipe (8), the constant temperature of the constant temperature heating box (51) is set to be 45-50 ℃, and the boiling point of the dimethyl disulfide is 109 ℃, the boiling point of the dimethyl trisulfide is 41 ℃, and the boiling point of the dimethyl tetrasulfide is higher than 243 ℃, so that the dimethyl disulfide liquid is evaporated when the dimethyl disulfide liquid flows through the inside of the constant temperature heating box (51), the dimethyl trisulfide doped in the dimethyl disulfide liquid is evaporated at 45 ℃, the evaporated dimethyl trisulfide steam is discharged to a condenser through the exhaust pipe (53) for condensation collection, the purity of the dimethyl disulfide liquid in the constant temperature heating box (51) can be further improved, and finally, the obtained high-purity dimethyl disulfide is discharged and collected through the exhaust pipe (52).
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