CN116751146B - Method for preparing prosulfocarb by using coking gas desulfurization and decyanation waste liquid - Google Patents
Method for preparing prosulfocarb by using coking gas desulfurization and decyanation waste liquid Download PDFInfo
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- CN116751146B CN116751146B CN202310740489.5A CN202310740489A CN116751146B CN 116751146 B CN116751146 B CN 116751146B CN 202310740489 A CN202310740489 A CN 202310740489A CN 116751146 B CN116751146 B CN 116751146B
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- kettle body
- material supporting
- supporting piece
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- prosulfocarb
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- 239000005603 Prosulfocarb Substances 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 46
- NQLVQOSNDJXLKG-UHFFFAOYSA-N prosulfocarb Chemical compound CCCN(CCC)C(=O)SCC1=CC=CC=C1 NQLVQOSNDJXLKG-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 239000007788 liquid Substances 0.000 title claims abstract description 20
- 238000006477 desulfuration reaction Methods 0.000 title claims abstract description 18
- 230000023556 desulfurization Effects 0.000 title claims abstract description 18
- 239000002699 waste material Substances 0.000 title claims abstract description 18
- 238000004939 coking Methods 0.000 title claims abstract description 13
- 238000007255 decyanation reaction Methods 0.000 title claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 148
- 239000011265 semifinished product Substances 0.000 claims abstract description 91
- 230000018044 dehydration Effects 0.000 claims abstract description 36
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 36
- 230000008569 process Effects 0.000 claims abstract description 28
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 238000005406 washing Methods 0.000 claims abstract description 12
- 239000003513 alkali Substances 0.000 claims abstract description 11
- 230000005587 bubbling Effects 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 239000000126 substance Substances 0.000 claims abstract description 6
- 238000007599 discharging Methods 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 230000009471 action Effects 0.000 claims description 8
- 239000000696 magnetic material Substances 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 abstract description 10
- 239000007789 gas Substances 0.000 description 21
- 238000006243 chemical reaction Methods 0.000 description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- WEHWNAOGRSTTBQ-UHFFFAOYSA-N dipropylamine Chemical compound CCCNCCC WEHWNAOGRSTTBQ-UHFFFAOYSA-N 0.000 description 4
- 239000000047 product Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- JFDZBHWFFUWGJE-UHFFFAOYSA-N benzenecarbonitrile Natural products N#CC1=CC=CC=C1 JFDZBHWFFUWGJE-UHFFFAOYSA-N 0.000 description 2
- KCXMKQUNVWSEMD-UHFFFAOYSA-N benzyl chloride Chemical compound ClCC1=CC=CC=C1 KCXMKQUNVWSEMD-UHFFFAOYSA-N 0.000 description 2
- 229940073608 benzyl chloride Drugs 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 2
- 238000006482 condensation reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 230000001739 rebound effect Effects 0.000 description 2
- 238000004904 shortening Methods 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 241000607479 Yersinia pestis Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000007259 addition reaction Methods 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- JFDZBHWFFUWGJE-KWCOIAHCSA-N benzonitrile Chemical group N#[11C]C1=CC=CC=C1 JFDZBHWFFUWGJE-KWCOIAHCSA-N 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000000295 fuel oil Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
- 239000002917 insecticide Substances 0.000 description 1
- 239000006193 liquid solution Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 239000012044 organic layer Substances 0.000 description 1
- 239000010815 organic waste Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
Classifications
-
- 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
- B01D3/34—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
- B01D3/343—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances the substance being a gas
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C333/00—Derivatives of thiocarbamic acids, i.e. compounds containing any of the groups, the nitrogen atom not being part of nitro or nitroso groups
- C07C333/02—Monothiocarbamic acids; Derivatives thereof
- C07C333/04—Monothiocarbamic acids; Derivatives thereof having nitrogen atoms of thiocarbamic groups bound to hydrogen atoms or to acyclic carbon atoms
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention relates to the technical field of prosulfocarb preparation, in particular to a method for preparing prosulfocarb by using coking gas desulfurization and decyanation waste liquid; the method comprises the following steps: s1: the raw materials are subjected to gas making, alkali washing, salifying and condensing processes to obtain a semi-finished product of prosulfocarb, and the semi-finished product enters the inside of the kettle body along the feed inlet; s2: the controller can control the heating component on the side wall of the kettle body to heat the kettle body, then the vacuum pump is started to pump away gaseous substances in the kettle body, and the controller can control the hydraulic cylinder to repeatedly extend and shorten, so that the semi-finished product is controlled to repeatedly drag upwards along the inner wall of the kettle body; s3: after the vacuum pump is used for vacuumizing, bubbling and dehydrating for 4-5 hours, discharging the finished prosulfocarb in the kettle body along a discharge hole; according to the invention, the semi-finished prosulfocarb is contacted with the invalid inner wall of the kettle body through the material supporting piece, so that the area of the semi-finished prosulfocarb transferred to the kettle body is enlarged, the vacuum bubbling dehydration efficiency of the semi-finished prosulfocarb is further improved, and the preparation efficiency of the finished prosulfocarb is improved.
Description
Technical Field
The invention relates to the technical field of prosulfocarb preparation, in particular to a method for preparing prosulfocarb by using coking gas desulfurization and decyanation waste liquid.
Background
Prosulfocarb is an insecticide produced by prosulfocarb agrochemical company and its main component is benzonitrile. It is widely used in agriculture, especially for preventing and controlling pests on rice, fruit tree and vegetable.
The desulfurization waste liquid refers to waste liquid generated after desulfurization treatment in industrial processes of coal, fuel oil or other sulfide-containing fuels. The preparation process of prosulfocarb can be realized by taking desulfurization waste liquid as an initial raw material, and the method comprises the steps of gas preparation, alkali washing, salifying, condensation and dehydration; the dehydration refers to transferring the semi-finished product of the middle tank to a dehydration kettle, maintaining the temperature at 90 ℃, and carrying out vacuumizing bubbling dehydration for 4-5h. And after the reaction is finished, the prosulfocarb raw medicine is obtained.
The temperature of the dehydration kettle can be increased under the heating state, so that heat is transferred to the internal semi-finished product, and along with the water vapor generated in the dehydration process of the semi-finished product, the quality of the semi-finished product in the dehydration kettle is reduced, so that the upper inner wall of the dehydration kettle is exposed, and the heat can be transferred to the semi-finished product only through the lower half part of the dehydration kettle, so that the dehydration efficiency of the semi-finished product is low, and the preparation efficiency of prosulfocarb is influenced.
In view of the above, the present invention provides a method for preparing prosulfocarb from coking gas desulfurization and decyanation waste liquid, which solves the above technical problems.
Disclosure of Invention
In order to make up the defects of the prior art, the invention provides a method for preparing prosulfocarb by using coking gas desulfurization and decyanation waste liquid.
The technical scheme adopted for solving the technical problems is as follows: the invention relates to a method for preparing prosulfocarb by using coking gas desulfurization and decyanation waste liquid, which comprises the following steps:
s1: the raw materials are subjected to gas making, alkali washing, salifying and condensing processes to obtain a semi-finished product of prosulfocarb, the semi-finished product enters the inside of a kettle body along a kettle body feed inlet in a dehydration kettle, and then the feed inlet is closed;
s2: a controller in the dehydration kettle controls a heating component on the side wall of the kettle body to heat the kettle body to 90 ℃, then a vacuum pump is started to pump away gaseous substances in the kettle body, and along with the repeated extension and shortening of a hydraulic cylinder in the water vapor flowing process generated in the dehydration process of the semi-finished product, the hydraulic cylinder drives a material supporting part to drag the semi-finished product upwards repeatedly along the inner wall of the kettle body;
s3: after the vacuum pump in the dehydration kettle is used for vacuumizing, bubbling and dehydrating for 4-5 hours, stopping the operation of the vacuum pump and the heating component, opening a discharge hole on the outer wall of the lower part of the kettle body, and discharging the finished prosulfocarb in the kettle body along the discharge hole;
wherein, dehydration cauldron that uses in S1-S3 includes:
a kettle body; the side wall of the kettle body is provided with a heating component, such as a resistance wire; the outer walls of the upper part and the lower part of the kettle body are respectively provided with a feed inlet and a discharge outlet and are controlled by valves;
a frame; the frame is fixedly connected to the lower half part of the kettle body;
a vacuum pump; the vacuum pump is fixedly connected to the outer wall of the kettle body and is used for vacuumizing the kettle body;
a hydraulic cylinder; the hydraulic cylinder is fixedly connected to the top of the kettle body, and an output shaft of the hydraulic cylinder extends into the kettle body;
a material supporting piece; the material supporting piece is positioned in the kettle body and is contacted with the inner wall of the kettle body; the material supporting piece is fixedly connected with the output shaft of the hydraulic cylinder through a cross rod;
a controller; the controller is used for controlling the automatic operation of the dehydration kettle.
Preferably, the material supporting piece is spiral; the spiral section of the material supporting piece is L-shaped; the vertical section part of the material supporting part is far away from the inner wall of the kettle body, and the transverse section part of the material supporting part is close to the inner wall of the kettle body and contacts with the inner wall of the kettle body; the material supporting piece has elasticity.
Preferably, the output shaft of the hydraulic cylinder is fixedly connected with a motor; an output shaft of the motor is connected with one end of the cross rod, which is far away from the material supporting piece; the motor is positioned at the center of the kettle body.
Preferably, the center of the inner bottom wall of the kettle body is fixedly connected with an inner column; an aggregate area is formed between the outer side wall of the inner column and the inner wall of the kettle body; the inner edge of the material supporting piece is contacted with the outer side wall of the inner column; the outer edge of the material supporting piece is contacted with the inner wall of the kettle body.
Preferably, one end of the material supporting piece, which is close to the upper part, is fixedly connected with the material guiding piece; one end of the material guide piece is communicated with one end of the material supporting piece, which is close to the upper end of the material supporting piece, and the other end of the material guide piece extends to the central shaft position of the kettle body.
Preferably, the material supporting piece consists of a vertical plate and a transverse plate; a baffle is arranged on the cross rod; one surface of the baffle close to the vertical plate is rotationally connected with the vertical plate through a rotating rod; the baffle is matched with the material supporting section of the material supporting piece; the baffle is arranged along the spiral direction of the material supporting piece; a magnet is arranged on the inner side of the kettle body and above the material supporting piece; the edge of the baffle, which is far away from the rotating rod, is made of magnetic materials.
Preferably, the rotating rod is rotationally connected with the vertical plate through a torsion spring; the rotating rod is fixedly connected with the baffle; the baffle is in a transverse state under the action of the torsion spring.
Preferably, the hydraulic cylinder output shaft is rotationally connected with the cross rod; a chute is arranged on the inner wall of the kettle body; the sliding chute is connected with the sliding block in a sliding way; the sliding block is connected with the bottom of the chute through a spring; and a first inclined plane is arranged at the lower position of one end of the sliding block, which is far away from the spring.
The beneficial effects of the invention are as follows:
1. according to the invention, the semi-finished prosulfocarb is contacted with the invalid inner wall of the kettle body through the material supporting piece, so that the area of the semi-finished prosulfocarb transferred to the kettle body is enlarged, the vacuum bubbling dehydration efficiency of the semi-finished prosulfocarb is further improved, and the preparation efficiency of the finished prosulfocarb is improved.
2. According to the invention, feeding can be realized under the condition of low water content and poor fluidity of the semi-finished product, and after the semi-finished product is fed by the material supporting piece, the hydraulic cylinder drives the motor to move upwards under the condition that the motor is kept to rotate continuously, so that the material supporting piece rotates continuously in an opening state, the semi-finished product can flow from bottom to top along the spiral line direction of the material supporting piece, the inner wall of the kettle body is completely covered by the semi-finished product, heat can be transmitted to the semi-finished product better, and quick dehydration of the semi-finished product is realized.
3. Under the condition that the material supporting piece rotates, the semi-finished product in the material collecting area moves upwards along the spiral line direction of the material supporting piece and flows out to the central shaft position of the kettle body along the material guiding piece and finally falls on the upper end of the inner column, the upper end of the inner column is arranged in a cone shape, so that the semi-finished product is scattered on the position of the material supporting piece under the rebound effect of the upper end of the inner column and moves upwards along the spiral line of the material supporting piece from bottom to top again, circulation is realized, and further, the semi-finished product is dehydrated more fully and uniformly.
Drawings
The invention will be further described with reference to the drawings and embodiments.
FIG. 1 is a flow chart of the method of the present invention;
FIG. 2 is a perspective view of example 1 of the present invention;
FIG. 3 is a perspective sectional view of example 2 of the present invention;
FIG. 4 is a block diagram of the guide of FIG. 3;
FIG. 5 is a perspective sectional view of example 3 of the present invention;
FIG. 6 is an enlarged view at A in FIG. 5;
FIG. 7 is a structural view of the baffle of FIG. 5;
fig. 8 is an enlarged view at B in fig. 7.
In the figure: kettle body 1, heating element 11, feed inlet 12, discharge gate 13, magnet 14, spout 15, slider 16, first inclined plane 161, spring 17, frame 2, vacuum pump 3, pneumatic cylinder 4, hold in the palm material piece 5, horizontal pole 51, riser 52, diaphragm 53, baffle 54, commentaries on classics stick 55, torsional spring 56, motor 6, interior post 7, gather materials district 71, guide 8.
Detailed Description
The invention is further described in connection with the following detailed description in order to make the technical means, the creation characteristics, the achievement of the purpose and the effect of the invention easy to understand.
As shown in fig. 1 to 8, the present invention is described in detail in the following embodiments:
example 1:
a method for preparing prosulfocarb by using coking gas desulfurization and decyanation waste liquid comprises the following steps:
s1: the raw materials are subjected to gas making, alkali washing, salifying and condensing processes to obtain a semi-finished product of prosulfocarb, the semi-finished product enters the inside of a kettle body 1 along a feed inlet 12 of the kettle body 1 in a dehydration kettle, and then the feed inlet 12 is closed;
s2: the controller in the dehydration kettle controls the heating component 11 on the side wall of the kettle body 1 to heat the kettle body 1 to 90 ℃, then the vacuum pump 3 is started to pump away gaseous substances in the kettle body 1, and along with the water vapor generated in the dehydration process of the semi-finished product, the controller controls the hydraulic cylinder 4 to repeatedly extend and shorten, and the hydraulic cylinder 4 drives the material supporting piece 5 to repeatedly drag the semi-finished product upwards along the inner wall of the kettle body 1;
s3: after the vacuum pump 3 in the dehydration kettle is vacuumized, bubbling and dehydrated for 4-5 hours, stopping the operation of the vacuum pump 3 and the heating component 11, opening a discharge hole 13 on the outer wall of the lower part of the kettle body 1, and discharging the finished prosulfocarb in the kettle body 1 along the discharge hole 13;
wherein, dehydration cauldron that uses in S1-S3 includes:
a kettle body 1; the side wall of the kettle body 1 is provided with a heating component 11, such as a resistance wire; the upper and lower outer walls of the kettle body 1 are respectively provided with a feed inlet 12 and a discharge outlet 13, and are controlled by valves;
a frame 2; the frame 2 is fixedly connected to the lower half part of the kettle body 1;
a vacuum pump 3; the vacuum pump 3 is fixedly connected to the outer wall of the kettle body 1 and is used for vacuumizing the kettle body 1;
a hydraulic cylinder 4; the hydraulic cylinder 4 is fixedly connected to the top of the kettle body 1, and an output shaft of the hydraulic cylinder 4 extends into the kettle body 1;
a material supporting member 5; the material supporting piece 5 is positioned in the kettle body 1, and the material supporting piece 5 is in contact with the inner wall of the kettle body 1; the material supporting piece 5 is fixedly connected with the output shaft of the hydraulic cylinder 4 through a cross rod 51;
a controller; the controller is used for controlling the automatic operation of the dehydration kettle;
when the dehydrating kettle is used, the temperature of the dehydrating kettle is increased in a heating state, so that heat is transferred to an internal semi-finished product, and along with the water vapor generated in the dehydrating process of the semi-finished product, the quality of the semi-finished product in the dehydrating kettle is reduced, the upper inner wall of the dehydrating kettle is exposed, and thus the heat can be transferred to the semi-finished product only through the lower half part of the dehydrating kettle, the dehydrating efficiency of the semi-finished product is low, and the preparation efficiency of prosulfocarb is influenced;
therefore, the invention firstly carries out the gas making reaction, the staff adds water into the enamel reaction kettle, then slowly drops sulfuric acid, controls the temperatureDropping desulfurization waste liquid solution into the kettle at the temperature lower than 50 ℃ under the reaction pressure of 0.031mPa for 4 hours to generate COS gas, wherein the equation of the gas preparation reaction is as follows: NH (NH) 4 SCN+2H 2 SO 4 +H 2 O→COS↑+2NH 4 HSO 4 Side reactions of NH may occur 4 SCN+2H 2 SO 4 +H 2 O→H 2 S+2NH 4 HSO 4 +CO 2 And 2NH 4 SCN+4H 2 SO 4 +2H 2 O→CS 2 +4NH 4 HSO 4 +CO 2 Then alkali washing is carried out, and a certain amount of 10% aqueous alkali is put into a closed gas washing kettle for washing; introducing COS gas generated by the reaction into a gas washing kettle, reacting for 4 hours at room temperature to obtain pure COS gas, wherein the reaction equation of alkaline washing reaction is as follows: h 2 SO 4 +2NaOH→Na 2 SO 4 +2H 2 O and H 2 S+2NaOH→Na 2 S+2H 2 O, COS gas can carry out a small amount of sulfuric acid, hydrogen sulfide and the like, and liquid alkali is used for absorption; then carrying out salification reaction, adding a certain amount of 32% liquid alkali and di-n-propylamine into a salification reaction kettle, and heating to 45 ℃; introducing COS gas to perform salification reaction for 4h to obtain N, N-di-N-propyl sodium thiocarbamate, and noticing CS 2 The content is not more than 0.2%, and CS 2 Is easier to react with di-N-propylamine than COS to generate N, N-di-N-propyl sodium dithiocarbamate, and the reaction equation of the salification reaction is as follows: COS+ (n-C) 3 H 7 ) 2 NH+NaOH→(n-C 3 H 7 ) 2 NCOSNa+H 2 O, a small amount of CS2 reacts with di-n-propylamine: CS (circuit switching) 2 +(n-C 3 H 7 ) 2 NH+NaOH→(n-C 3 H 7 ) 2 NCS 2 Na+H 2 O, then carrying out condensation reaction, adding a certain amount of benzyl chloride into a salifying reaction kettle, controlling the temperature to be 60-70 ℃, stirring for 20min, after reacting for 4h, preserving heat for 2.5h, adding a proper amount of water and hydrochloric acid to adjust the PH, standing and layering for 3h, wherein the total reaction time is 12h, putting the lower organic layer into a middle tank, and the condensation reaction equation is as follows: (n-C) 3 H 7 ) 2 NCOSNa+C 6 H 5 CH 2 Cl→(n-C 3 H 7 ) 2 NCOSCH 2 (C 6 H 5 ) +NaCl, finally, the semi-finished product of the middle tank enters the kettle body 1 along the feed inlet 12 of the kettle body 1, then the feed inlet 12 is closed, the controller controls the heating component 11 on the side wall of the kettle body 1 to heat the kettle body 1, the temperature of the kettle body 1 is heated to about 90 ℃, the vacuum pump 3 is started to pump away the gaseous substances in the kettle body 1, the gaseous substances comprise air, water vapor, organic waste gas and the like, the semi-finished product quality in the kettle body 1 is reduced along with the water vapor flow away generated in the dehydration process of the semi-finished product, the upper inner wall of the kettle body 1 is exposed, the heat of the kettle body 1 can only be transferred to the semi-finished product in the kettle body 1 through the lower half part, so the controller can control the repeated extension and shortening of the hydraulic cylinder 4, the extension process of the hydraulic cylinder 4 can drive the material supporting part 5 to move downwards, the material supporting part 5 can be contacted with the semi-finished product in the lower half part of the kettle body 1 after moving downwards, the semi-finished product falls on the material supporting part 5, then the hydraulic cylinder 4 shortens and drives the material supporting part 5 to move upwards under the condition of supporting part semi-finished product, the material supporting part 5 can drag part of the semi-finished product upwards along the inside of the kettle body 1, the part of the semi-finished product in the static state in the kettle body 1, which is contacted with the inner wall of the kettle body 1, is an effective inner wall, the part of the semi-finished product in the static state in the kettle body 1, which is not contacted with the inner wall of the kettle body 1, is an ineffective inner wall, obviously, the ineffective side wall is above the effective side wall, the semi-finished product can transfer heat into the semi-finished product on the material supporting part 5 after the ineffective inner wall of the kettle body 1 is stored under the driving of the material supporting part 5, the semi-finished product on the material supporting part 5 can be dehydrated quickly, the heat can be transferred to the semi-finished product in the kettle body 1 more quickly, the contact area of the inner wall of the kettle body 1 and the semi-finished product is increased, the dehydration efficiency of the semi-finished product is improved, the expansion and contraction of the hydraulic cylinder 4 are repeatedly carried out, after the vacuumizing bubbling dehydration is carried out for 4-5 hours, the finished prosulfocarb is obtained after the reaction is finished, and finally, a discharge hole 13 on the outer wall of the lower part of the kettle body 1 is opened, and the finished prosulfocarb is discharged along the discharge hole 13;
according to the invention, the semi-finished prosulfocarb is contacted with the invalid inner wall of the kettle body 1 through the material supporting piece 5, so that the area of the semi-finished prosulfocarb transferred into the kettle body 1 is enlarged, the vacuum bubbling dehydration efficiency of the semi-finished prosulfocarb is further improved, and the preparation efficiency of the finished prosulfocarb is improved.
In this embodiment, the material supporting member 5 is spiral; the spiral section of the material supporting piece 5 is L-shaped; the vertical section part of the material supporting piece 5 is far away from the inner wall of the kettle body 1, and the transverse section part of the material supporting piece 5 is close to the inner wall of the kettle body 1 and contacts with the inner wall of the kettle body 1; the material supporting piece 5 has elasticity;
when in use, the hydraulic cylinder 4 can repeatedly stretch in the vacuum bubbling dehydration process of the semi-finished product in the kettle body 1, the hydraulic cylinder 4 can drive the cross rod 51 to move downwards in the stretching process, the cross rod 51 can extrude the upper end of the material supporting piece 5 to move downwards in the downward moving process, so that the material supporting piece 5 is compressed, the screw pitch of the material supporting piece 5 is reduced, the height of the material supporting piece 5 is shortened in the whole extruding process, the material supporting piece 5 can enter the inner side of the effective inner wall of the kettle body 1 and is contacted with the semi-finished product in the kettle body 1, the material supporting piece 5 is formed by combining a vertical plate 52 and a transverse plate 53, the semi-finished product can fall on the upper end of the transverse plate 53 of the material supporting piece 5 and the outer side of the vertical plate 52, then the hydraulic cylinder 4 can drive the cross rod 51 to move upwards, the cross rod 51 can enable the material supporting piece 5 to be converted from a compressed state to a propped state, the material supporting piece 5 can drive the supported semi-finished product to move upwards in the propped state in the stretching process, the semi-finished product supported by the supporting piece 5 is contacted with the invalid inner wall of the kettle body 1 in the upward moving process, the temperature on the invalid inner wall of the kettle body 1 is transferred into the semi-finished product on the supporting piece 5, the semi-finished product is supported by the supporting piece 5 to move upward, the semi-finished product slides down along the upper end of the transverse plate 53 in the supporting piece 5 under the action of gravity and along the spiral direction of the supporting piece 5, the semi-finished product is contacted with the invalid inner wall of the kettle body 1 in the sliding process of the supporting piece 5, the heat transfer range is enlarged, after the semi-finished product on the supporting piece 5 moves down to the inner side of the valid inner wall of the kettle body 1 along the spiral direction of the supporting piece 5, the hydraulic cylinder 4 shortens and drives the transverse rod 51 to move downward, the transverse rod 51 is connected with the position on which the supporting piece 5 is positioned, the downward movement of the transverse rod 51 can drive the supporting piece 5 to compress again, so that the semi-finished product on the inner side of the effective inner wall of the kettle body 1 is repeatedly conveyed to be in contact with the ineffective inner wall of the kettle body 1.
Example 2, this example is directed to the case where the semi-finished product has less moisture and poor fluidity:
the output shaft of the hydraulic cylinder 4 is fixedly connected with a motor 6; an output shaft of the motor 6 is connected with one end of the cross rod 51 far away from the material supporting piece 5; the motor 6 is positioned at the center of the kettle body 1;
when the semi-finished product dewatering device is used, the hydraulic cylinder 4 drives the cross rod 51 to move downwards to the limit position, the controller can control the motor 6 to rotate, the rotating motor 6 can drive the cross rod 51 to rotate around the output shaft of the motor 6, the cross rod 51 can drive the material supporting plate to synchronously rotate under the drive, so that the material supporting plate is controlled to rotate along the spiral direction, one end of the material supporting plate is propped against the lower side wall of the kettle body 1, so that the material supporting plate can shovel a semi-finished product into the material supporting position of the material supporting plate in the rotating process, compared with the prior material supporting plate which moves downwards directly to realize semi-finished product feeding, the embodiment can realize feeding under the condition that the semi-finished product has less water and poor fluidity, and after the semi-finished product feeding is completed, the material supporting member 5 continues to rotate under the condition that the motor 6 is kept, the hydraulic cylinder 4 drives the motor 6 to move upwards, so that the material supporting member 5 continues to rotate in the stretching state, so that the inner wall of the kettle body 1 can be completely covered by the semi-finished product along the spiral direction of the material supporting member 5, so that the heat can be transferred to the semi-finished product is quickly dehydrated; in the spiral rising process of the semi-finished product is realized by the rotation of the motor 6, the hydraulic cylinder 4 can repeatedly stretch, so that the material supporting piece 5 is repeatedly compressed and stretched, the semi-finished product can be overturned by the material supporting piece 5, and the steam of the semi-finished product can be quickly lost.
In the embodiment, the center of the inner bottom wall of the kettle body 1 is fixedly connected with an inner column 7; an aggregate area 71 is formed between the outer side wall of the inner column 7 and the inner wall of the kettle body 1; the inner edge of the material supporting piece 5 is contacted with the outer side wall of the inner column 7; the outer edge of the material supporting piece 5 is in contact with the inner wall of the kettle body 1;
when the semi-finished product collecting device is used, the center of the inner bottom wall of the kettle body 1 is fixedly connected with the inner column 7, so that an aggregate area 71 is formed between the outer side wall of the inner column 7 and the inner wall of the kettle body 1, the upper end surface of the inner column 7 is conical, so that the semi-finished product can fall in the aggregate area 71 in a concentrated manner, and the semi-finished product in the aggregate area 71 can be moved upwards in a spiral manner by the material supporting piece 5 more easily along with the rotation of the material supporting piece 5; the discharge hole 13 of the kettle body 1 is communicated with the material collecting area 71, so that under the condition of discharging, the motor 6 is reversely rotated to drive the material supporting piece 5 to reversely rotate, the material supporting piece 5 reversely rotates to enable a finished product to flow into the material collecting area 71 from top to bottom, and along with the continuous rotation of the material supporting piece 5, the finished product in the material collecting area 71 is extruded by the material supporting piece 5 along the discharge hole 13 of the kettle body 1, so that the discharge efficiency of the prosulfocarb of the finished product is improved.
In this embodiment, one end of the material supporting member 5, which is close to the upper end, is fixedly connected with a material guiding member 8; one end of the material guide piece 8 is communicated with one end of the material supporting piece 5, which is close to the upper end, and the other end of the material guide piece extends to the central shaft position of the kettle body 1;
when the semi-finished product collecting device is used, under the condition that the material supporting piece 5 rotates, the semi-finished product in the material collecting area 71 moves upwards along the spiral line direction of the material supporting piece 5 and flows out to the central shaft position of the kettle body 1 along the material guiding piece 8, finally falls on the upper end of the inner column 7, and the upper end of the inner column 7 is arranged in a conical shape, so that the semi-finished product is scattered on the position of the material supporting piece 5 under the rebound effect of the upper end of the inner column 7 and moves upwards along the spiral line of the material supporting piece 5 from bottom to top again, and the circulation is realized, so that the semi-finished product is dehydrated more fully and uniformly.
Example 3, this example is directed to the case where the semi-finished product has a large water content and a high fluidity:
the material supporting piece 5 consists of a vertical plate 52 and a transverse plate 53; a baffle 54 is arranged on the cross rod 51; one surface of the baffle 54, which is close to the vertical plate 52, is rotatably connected with the vertical plate 52 through a rotating rod 55; the baffle 54 is matched with the material supporting section of the material supporting piece 5; the baffle plate 54 is arranged along the spiral direction of the material supporting piece 5; a magnet 14 is arranged on the inner side of the kettle body 1 and above the material supporting piece 5; the edge of the baffle 54 away from the rotating rod 55 is made of magnetic material;
when the device is used, the hydraulic cylinder 4 is shortened, so that the screw pitch of the material supporting piece 5 is increased in the process of supporting the material supporting piece 5 under the action of self elasticity, the material supporting piece 5 can drive the baffle 54 to move close to the magnet 14, the baffle 54 is closer to the magnet 14 along with the driving of the material supporting piece 5, the larger the magnetic force born by the baffle 54 is, the edge of the baffle 54 far away from the rotating rod 55 is made of a magnetic material, the baffle 54 overcomes the gravity of the baffle 54 to drive the rotating rod 55 and rotates around the central shaft of the rotating rod 55 under the action of the magnetic force, the baffle 54 can be converted from a transverse state to a vertical state under the action of the magnetic force, so that the semi-finished product on the material supporting plate is received, the baffle 54 can be arranged in a plurality of along the spiral line direction of the material supporting piece 5, so that more semi-finished products are blocked by the baffle 54, the loss and the running speed of the semi-finished product are reduced in the process of supporting the material supporting and the upper moving of the material supporting piece 5, the contact time of the semi-finished product and the invalid inner wall of the kettle body 1 is further improved, and the heat transfer effect is indirectly improved; under the condition that the baffle plate 54 is far away from the magnet 14 along with the material supporting plate, the baffle plate 54 is pushed away to be in a transverse state under the flow of the semi-finished product, so that the semi-finished product on the material supporting piece 5 falls into the lower half part of the kettle body 1 in advance before the material supporting piece 5 is compressed to the limit position, and the mixed semi-finished product is supported by the material supporting piece 5.
In this embodiment, the rotating rod 55 is rotatably connected to the riser 52 by a torsion spring 56; the rotating rod 55 is fixedly connected with the baffle 54; the baffle 54 is in a transverse state under the action of a torsion spring 56;
when the device is used, due to the action of the torsion spring 56, the baffle 54 can be changed into a vertical state from a transverse state by the magnet 14 when the magnet 14 needs to additionally overcome the torsion force of the torsion spring 56 in the process of moving the material supporting piece 5 upwards, the semi-finished product on the material supporting piece 5 is intercepted, and the baffle 54 can be squeezed out to realize the transition of the transverse state by the baffle 54 under the torsion force of the torsion spring 56 when the baffle 54 is kept away from the magnet 14 along with the material supporting piece 5, so that the semi-finished product around the baffle 54 is prevented from blocking the smooth transition of the transverse state of the baffle 54.
In this embodiment, the output shaft of the hydraulic cylinder 4 is rotatably connected with the cross rod 51; a chute 15 is arranged on the inner wall of the kettle body 1; the sliding groove 15 is connected with a sliding block 16 in a sliding way; the sliding block 16 is connected with the bottom of the chute 15 through a spring 17; a first inclined surface 161 is arranged at the lower position of one end of the sliding block 16 far away from the spring 17;
when the feeding device is used, in the process that the hydraulic cylinder 4 drives the cross rod 51 to move upwards, the material supporting piece 5 can extrude the first inclined plane 161, the first inclined plane 161 on the sliding block 16 can overcome the movement of the spring 17 towards the bottom of the sliding groove 15 when being extruded, so that the sliding block 16 is retracted into the sliding groove 15, the material supporting piece 5 can be spread smoothly, in the process that the hydraulic cylinder 4 drives the cross rod 51 to move downwards, the material supporting piece 5 can be blocked by the sliding block 16, and because the cross rod 51 is rotationally connected with the output shaft of the hydraulic cylinder 4, the material supporting piece 5 can rotate along the spiral line direction under the blocking of the sliding block 16, the semi-finished product on the inner side of the effective inner wall of the kettle body 1 can be disturbed in the rotation process of the material supporting piece 5, the mixing is realized, and the feeding is realized smoothly after the material supporting piece 5 is compressed.
Example 4:
the desulfurization waste liquid is used as an initial raw material, and reacts with sulfuric acid and water to generate gas COS, the gas COS is subjected to alkali liquor washing, then undergoes addition reaction and neutralization reaction with liquid alkali and di-N-propylamine to generate N, N-di-N-propyl thiocarbamic acid sodium salt, sodium salt and benzyl chloride, and undergoes double decomposition reaction to generate crude prosulfocarb, and the crude prosulfocarb is obtained through a water washing procedure.
In the description of the present invention, it should be noted that the terms "center", "longitudinal", "lateral", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in fig. 1, are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the apparatus or element in question must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the scope of the present invention, and furthermore, the terms "first", "second", "third", etc. are merely used for distinguishing the description, and should not be construed as indicating or implying relative importance.
The foregoing has shown and described the basic principles, principal features and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (5)
1. A method for preparing prosulfocarb by using coking gas desulfurization and decyanation waste liquid is characterized in that: the method comprises the following steps:
s1: the raw materials are subjected to gas making, alkali washing, salifying and condensing processes to obtain a semi-finished product of prosulfocarb, the semi-finished product enters the inside of a kettle body (1) along a feed inlet (12) of the kettle body (1) in a dehydration kettle, and then the feed inlet (12) is closed;
s2: a controller in the dehydration kettle can control a heating component (11) on the side wall of the kettle body (1) to heat the kettle body (1) to 90 ℃, then a vacuum pump (3) is started to pump away gaseous substances in the kettle body (1), and the controller can control a hydraulic cylinder (4) to repeatedly extend and shorten along with the water vapor flowing away process generated in the dehydration process of the semi-finished product, and the hydraulic cylinder (4) can drive a material supporting part (5) to repeatedly drag the semi-finished product upwards along the inner wall of the kettle body (1);
s3: after a vacuum pump (3) in the dehydration kettle is vacuumized, bubbling and dehydrated for 4-5 hours, stopping the operation of the vacuum pump (3) and a heating component (11), opening a discharge hole (13) on the outer wall of the lower part of the kettle body (1), and discharging the finished prosulfocarb in the kettle body (1) along the discharge hole (13);
wherein, dehydration cauldron that uses in S1-S3 includes:
a kettle body (1); a heating component (11) is arranged on the side wall of the kettle body (1); the upper part and the lower part of the kettle body (1) are respectively provided with a feed inlet (12) and a discharge outlet (13) and are controlled by valves;
a frame (2); the frame (2) is fixedly connected to the lower half part of the kettle body (1);
a vacuum pump (3); the vacuum pump (3) is fixedly connected to the outer wall of the kettle body (1) and is used for vacuumizing the kettle body (1);
a hydraulic cylinder (4); the hydraulic cylinder (4) is fixedly connected to the top of the kettle body (1), and an output shaft of the hydraulic cylinder (4) extends into the kettle body (1);
a material supporting piece (5); the material supporting piece (5) is positioned in the kettle body (1), and the material supporting piece (5) is in contact with the inner wall of the kettle body (1); the material supporting piece (5) is fixedly connected with the output shaft of the hydraulic cylinder (4) through a cross rod (51);
a controller; the controller is used for controlling the automatic operation of the dehydration kettle;
the material supporting piece (5) is spiral; the spiral section of the material supporting piece (5) is L-shaped; the vertical section of the material supporting piece (5) is far away from the inner wall of the kettle body (1), and the transverse section of the material supporting piece (5) is close to the inner wall of the kettle body (1) and is in contact with the inner wall of the kettle body (1); the material supporting piece (5) has elasticity;
an output shaft of the hydraulic cylinder (4) is fixedly connected with a motor (6); an output shaft of the motor (6) is connected with one end of the cross rod (51) far away from the material supporting piece (5); the motor (6) is positioned at the center of the kettle body (1);
the material supporting piece (5) consists of a vertical plate (52) and a transverse plate (53); a baffle (54) is arranged on the cross rod (51); one surface of the baffle plate (54) close to the vertical plate (52) is rotationally connected with the vertical plate (52) through a rotating rod (55); the baffle (54) is matched with the material supporting section of the material supporting piece (5); the baffle (54) is arranged along the spiral direction of the material supporting piece (5); a magnet (14) is arranged on the inner side of the kettle body (1) and above the material supporting piece (5); the edge of the baffle plate (54) far away from the rotating rod (55) is made of magnetic materials.
2. The method for preparing prosulfocarb by using coking gas desulfurization and decyanation waste liquid according to claim 1, which is characterized in that: the center of the inner bottom wall of the kettle body (1) is fixedly connected with an inner column (7); an aggregate area (71) is formed between the outer side wall of the inner column (7) and the inner wall of the kettle body (1); the inner edge of the material supporting piece (5) is contacted with the outer side wall of the inner column (7); the outer edge of the material supporting piece (5) is contacted with the inner wall of the kettle body (1).
3. The method for preparing prosulfocarb by using coking gas desulfurization and decyanation waste liquid according to claim 2, which is characterized in that: one end of the material supporting piece (5) close to the upper part is fixedly connected with a material guiding piece (8); one end of the material guide piece (8) is communicated with one end of the material supporting piece (5) which is close to the upper part, and the other end of the material guide piece extends to the central shaft position of the kettle body (1).
4. The method for preparing prosulfocarb by using coking gas desulfurization and decyanation waste liquid according to claim 1, which is characterized in that: the rotating rod (55) is rotationally connected with the vertical plate (52) through a torsion spring (56); the rotating rod (55) is fixedly connected with the baffle (54); the baffle plate (54) is in a transverse state under the action of a torsion spring (56).
5. The method for preparing prosulfocarb by using coking gas desulfurization and decyanation waste liquid according to claim 4, which is characterized in that: the output shaft of the hydraulic cylinder (4) is rotationally connected with the cross rod (51); a chute (15) is arranged on the inner wall of the kettle body (1); the sliding groove (15) is connected with a sliding block (16) in a sliding way; the sliding block (16) is connected with the bottom of the chute (15) through a spring (17); a first inclined surface (161) is arranged at the lower position of one end, far away from the spring (17), of the sliding block (16).
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Citations (5)
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|---|---|---|---|---|
| EP0697402A1 (en) * | 1994-08-19 | 1996-02-21 | Monsanto Europe S.A./N.V. | Manufacturing process for the production of prosulfocarb |
| CN108997181A (en) * | 2018-08-28 | 2018-12-14 | 陕西恒润化学工业有限公司 | A kind of prosulfocarb and its synthetic method |
| CN209944926U (en) * | 2019-03-13 | 2020-01-14 | 辛集市玺宸热能有限公司 | A dehydration cauldron for methyl benzotriazole production |
| CN114685334A (en) * | 2020-12-28 | 2022-07-01 | 南通泰禾化工股份有限公司 | Preparation method of prosulfocarb |
| CN115253974A (en) * | 2022-08-10 | 2022-11-01 | 甘肃德通医药化学技术有限公司 | Dehydration kettle for piperazine compound production and working method thereof |
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2023
- 2023-06-21 CN CN202310740489.5A patent/CN116751146B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0697402A1 (en) * | 1994-08-19 | 1996-02-21 | Monsanto Europe S.A./N.V. | Manufacturing process for the production of prosulfocarb |
| CN108997181A (en) * | 2018-08-28 | 2018-12-14 | 陕西恒润化学工业有限公司 | A kind of prosulfocarb and its synthetic method |
| CN209944926U (en) * | 2019-03-13 | 2020-01-14 | 辛集市玺宸热能有限公司 | A dehydration cauldron for methyl benzotriazole production |
| CN114685334A (en) * | 2020-12-28 | 2022-07-01 | 南通泰禾化工股份有限公司 | Preparation method of prosulfocarb |
| CN115253974A (en) * | 2022-08-10 | 2022-11-01 | 甘肃德通医药化学技术有限公司 | Dehydration kettle for piperazine compound production and working method thereof |
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