Thiofide 2-mercapto benzothiazole totally enclosed production system
Technical field
The invention belongs to thiofide 2-mercapto benzothiazole production technical field, be specifically related to a kind of thiofide 2-mercapto benzothiazole totally enclosed clean-production system.
Background technology
Thiofide 2-mercapto benzothiazole (MBT) is widely used a kind of universal promotor in the rubber industry, is the maximum product of at present domestic and international thiofide volume of production and marketing, also is simultaneously the main raw material of producing other promotor.High-content MBT still produces the main raw material of cephalosporin analog antibiotic medicine.But the MBT purity that high pressure is synthesized is low, contains plurality of impurities (being referred to as resin), can not directly use.Therefore, the refining purification process of MBT becomes a very important step in its production.The working method of present domestic rubber vulcanization accelerant MBT has two kinds: the one, and the soda acid WATER-WASHING METHOD; The 2nd, solvent extration.The soda acid WATER-WASHING METHOD is present domestic the most frequently used process for refining and purifying, accounts for dominant position.This method will consume a large amount of strong acid, highly basic and water, produces product per ton and can produce the high density saliferous organic basic waste water more than 45 tons, the aftertreatment difficulty.Solvent extration is present more novel process for refining and purifying.Along with the increasing of environmental protection dynamics, refining purification techniques of solvent extration and anhydrous process more and more receive people's attention.The solvent that existing solvent method uses is main with toluene mainly.Its operational path is following:
(1) height is pressed into: with HPP aniline that measures (400 kilograms) and three nitric sulfids (245 kilograms of 400 kilograms+Sulfurs of dithiocarbonic anhydride) are squeezed into the high pressure synthesis reactor successively; Close relevant charging valve on the still; Open the outside electric heater of kettle, feeding temperature-raising.When temperature in the kettle reaches 210 ~ 220 ℃, when pressure reaches 2.0-2.2MPa, closes electric heater, stop to send.When temperature of charge, pressure no longer change in the still, continue to prolong soaking time, when temperature in the kettle drops to 220 ℃, open pressure relief valve, keep relief pipeline internal pressure 0.055-0.06MPa, be zero until the still internal pressure.
(2) crystallization extracts: the MBT that dissolves after will synthesizing with the 0.03MPa saturation steam is pressed in the uncovered type crystallizer tank; Open the crystallizer tank Cold water tap and feed the cold water cooling to the cell wall chuck; After treating the complete crystallization of material; Artificial with crystallized stock dig out, fragmentation, and with in the disposable input extraction kettle of the thick MBT crystallized stock of about 700 kilograms/still.Open toluene injection valve on the extraction kettle, in the disposable adding extraction kettle of 2000 liters of toluene that has measured, soak after 45 minutes, open extraction kettle and stir, carry out the washing extraction first time, keep stirring and shut down static after 30 minutes.After static 60 minutes stratified supernatant, line strainer is put into mother liquor tank after filtering.Open toluene injection valve on the extraction kettle, in the disposable adding extraction kettle of 1500 liters of toluene that has measured, open extraction kettle and stir, carry out the washing extraction second time, keep stirring and shut down static after 30 minutes.After static 60 minutes stratified supernatant, line strainer is put into mother liquor tank after filtering.Open toluene injection valve on the extraction kettle, in the disposable adding extraction kettle of 1000 liters of toluene that has measured, open extraction kettle and stir; Wash extraction for the third time; Keep and stir after 30 minutes, open extraction kettle bottom dispensing valve material is put into uncovered type vacuum filtration groove, simultaneously open vacuum suction filtration trench bottom discharge port; Utilize vacuum that supernatant is evacuated in the mother liquor tank, generation crack, material surface can stop vacuum filtration in groove.
(3) drying and crushing and packing: bipyramid is circled round after drying machine comes to a complete stop, opens people from top orifice plate lid, after material in the suction filtration groove (about 570 kilograms) pack, disposable throw circle round drying machine to bipyramid in, close people from top orifice plate lid.Open the bipyramid drying machine that circles round, open body axial region admission valve and feed the 0.035-0.05MPa saturation steam, open body axial region vacuum valve to the body external jacket.Observe that the toluene in the visor distillates situation on the body vacuum pipe, when no toluene distillates with body in temperature rise to 120 ℃, shut down after 30 minutes, open bipyramid drying machine people from bottom orifice plate lid that circles round, material is put to charging tray and is packed.Mass transport is pulverized and packed, puts in storage after pulverizing the room.
This shows shortcoming such as the technology of existing SX purification 2-mercapto benzothiazole is the opened type manual operation, and extraction solvent evaporates in the air, has severe operational environment, and labour intensity is big.
Summary of the invention
The objective of the invention is to solve the above-mentioned technical problem that exists in the prior art, a kind of thiofide 2-mercapto benzothiazole totally enclosed clean-production system is provided.
For realizing above-mentioned purpose, the technical scheme that the present invention adopts is following:
Thiofide 2-mercapto benzothiazole totally enclosed clean-production system of the present invention comprises the high pressure synthesis system, crude product purification system and exhaust treatment system; Described crude product purification system comprises extraction kettle; 2-mercapto benzothiazole bullion directly pumps into extraction kettle from the high pressure synthesis reactor, and the 2-mercapto benzothiazole outlet of extraction kettle is connected with drying machine, and the mother liquor outlet of extraction kettle connects mother liquor holding tank; Mother liquor holding tank is connected with rectifying tower; The rectifying tower top connects toluene tank, and the toluene of recovery inserts extraction kettle through the toluene test tank, and the rectifier bottoms discharge port is connected with resin storage tank.
Described extraction kettle comprises kettle, is provided with whipping appts at the kettle top, is provided with spraying gun on kettle top; Be provided with filtering net in the kettle bottom, constitute the mother liquor chamber between at the bottom of filtering net and the still, autoclave body bottom is provided with the mother liquor outlet and exports with the 2-mercapto benzothiazole; The mother liquor outlet is connected with mother liquor holding tank; The outlet of 2-mercapto benzothiazole is connected with drying machine, outside kettle, is provided with chuck, and chuck is provided with cooling water inlet and cooling water outlet.
Described spraying gun comprises the spraying gun housing, is provided with the spraying gun shower nozzle in case top, and shower nozzle is provided with toluene feed mouth and 2-mercapto benzothiazole opening for feed; Housing top is provided with the oxygen level test port, and housing sidewall is provided with vacuum orifice, adds nitrogen mouth and venting, and housing bottom is provided with discharge port.
Described spraying gun shower nozzle comprises head body, is provided with the toluene liquid-inlet pipe that is communicated with the toluene feed mouth on head body top, and the toluene liquid-inlet pipe is communicated with the toluene film forming chamber; Described toluene film forming chamber is cylindric; On the sidewall of head body, be provided with the 2-mercapto benzothiazole liquid-inlet pipe that is communicated with 2-mercapto benzothiazole opening for feed, 2-mercapto benzothiazole liquid-inlet pipe is communicated with 2-mercapto benzothiazole film forming chamber, and described 2-mercapto benzothiazole film forming chamber is cylindric; Toluene liquid film forming chamber bottom is connected with 2-mercapto benzothiazole film forming chamber bottom, and described toluene film forming chamber bottom is a conically shaped with the place of being connected, 2-mercapto benzothiazole film forming chamber bottom; The head body bottom is provided with mixture export.
Described drying machine comprises dry chamber, and dry chamber roof is provided with opening for feed, and the bottom is provided with discharge port; Indoor stir shaft and the agitating vane that is provided with by drive power source of drying chamber; It is characterized in that: described stir shaft is hollow stir shaft, and the top is provided with steam inlet and vapour outlet, and said agitating vane is spiral double-deck agitating vane; The two-layer inner chamber of agitating vane is connected with steam inlet and vapour outlet respectively, and two-layer agitating vane bottom links; Be provided with interlayer at the drying chamber chamber outer wall, interlayer is provided with inlet mouth and air outlet.
Described high pressure synthesis system comprises the high pressure synthesis reactor, and the aniline storage tank is connected with the high pressure synthesis reactor through the aniline test tank, and the dithiocarbonic anhydride storage tank is connected with sulfur melting kettle, and sulfur melting kettle is connected with the high pressure synthesis reactor with molten sulphur liquid test tank through dissolving the sulphur liquid storage tank successively.
Described exhaust treatment system comprises the one-level tourie; The vapor pipe of one-level tourie connects the dithiocarbonic anhydride holding tank; Dithiocarbonic anhydride holding tank bottom connects the dithiocarbonic anhydride storage tank; The vapor pipe of dithiocarbonic anhydride holding tank connects secondary tourie, three grades of touries and level Four tourie successively, and touries at different levels all connect sulphur hydrogen flower sodium storage tank.
Totally-enclosed cleaner production purification system of the present invention is on the basis of former SX method of purification, utilizes the technical matters of independent research and equipment to carry out the novelty improvement, mainly shows two aspects: the one, and high low temperature exchanges cold abstraction technique.With a pair of horses going side by side of high-temperature liquid state (180-220 ℃) the crude 2-mercapto benzene after synthetic thiazole in autoclave with in nitrogen pressure to the airtight self-control extraction kettle; Directly carry out high low temperature at spraying gun shower nozzle internal spraying Cheng Fenyu toluene (normal temperature) and exchange extraction; Thereby improved the solubleness of resin in toluene, and stablized the fineness of MBT.High low temperature exchanges cold abstraction technique and has not only improved the extraction precision, has also thoroughly solved the blast problem of toluene steam and air mixture, has realized the technical renovation of being shifted to closed-loop operation by uncovered type manual operation fully.The 2nd, suction filtration, drying integrated technology.Utilize potential difference to realize accomplishing suction filtration oven dry operation in the upright three-dimensional helicoid screw dryer of automatic discharging to airtight self-control the M after the extraction with suction filtration, drying function.Suction filtration, drying integrated technology have not only realized closed-loop operation, have also alleviated the labour intensity in the technological operation greatly, and above-mentioned 2 is that the whole piece operational path is realized totally-enclosed leak free core technology.Organic solvent totally-enclosed cleaner production purifying technique does not have outside the advantage of spent process water discharging having kept the SX method of purification, has solved the vivid degree of 2-mercapto benzothiazole product appearance deficiency that former technology exists, severe operational environment, shortcoming that labour intensity is big.Overcome pollution that uncovered cooling, uncovered suction filtration bring environment and to operator's harm; Overcome extraction with dry by the manual work drawback with discharging that feeds intake, realized that fully airtight discharging, airtight extraction, airtight suction filtration are dry, really accomplished the totally-enclosed nothing leakage serialization production of no organic gas discharging.
Description of drawings
Fig. 1 is a structural representation of the present invention.
Fig. 2 is the structural representation of extraction kettle among the present invention.
Fig. 3 is the structural representation of spraying gun among the present invention.
Fig. 4 is the structural representation of spraying gun shower nozzle among the present invention.
Fig. 5 is the structural representation of drying machine among the present invention.
Fig. 6 is the vertical view of the stir shaft of drying machine among the present invention.
Embodiment
Thiofide 2-mercapto benzothiazole totally enclosed clean-production system of the present invention is as shown in Figure 1, comprises high pressure synthesis system 1, crude product purification system 2 and exhaust treatment system 3; Described crude product purification system comprises extraction kettle 4; 2-mercapto benzothiazole bullion directly pumps into extraction kettle 4 from high pressure synthesis reactor 17, and the 2-mercapto benzothiazole outlet of extraction kettle (4) is connected with drying machine 7, and the mother liquor outlet of extraction kettle connects mother liquor holding tank (8); Mother liquor holding tank 8 is connected with rectifying tower 9; Rectifying tower 9 tops connect toluene tank 11, and the toluene of recovery inserts extraction kettle 4 through toluene test tank 5, and rectifying tower 9 bottom discharge mouths are connected with resin storage tank 10.
Described extraction kettle is as shown in Figure 2, comprises kettle, is provided with whipping appts 4-3 at the kettle top; Be provided with spraying gun 4-2 on kettle top; Be provided with filtering net 4-6 in the kettle bottom, constitute mother liquor chamber 4-9 between at the bottom of filtering net 4-6 and the still, autoclave body bottom is provided with mother liquor outlet 4-7 and exports 4-8 with the 2-mercapto benzothiazole; Mother liquor outlet 4-7 is connected with mother liquor holding tank 8; 2-mercapto benzothiazole outlet 4-8 is connected with drying machine 7, outside kettle, is provided with chuck 4-5, and chuck 4-5 is provided with cooling water inlet 4-10 and cooling water outlet 4-1.
Described spraying gun is as shown in Figure 3, comprises spraying gun housing 38, is provided with spraying gun shower nozzle 36 at housing 38 tops, and shower nozzle 36 is provided with toluene feed mouth 35 and 2-mercapto benzothiazole opening for feed 34; Housing top is provided with oxygen level test port 33, and housing sidewall is provided with vacuum orifice 32, adds nitrogen mouth 31 and venting 37, and housing 38 bottoms are provided with discharge port 39.
Described spraying gun shower nozzle is as shown in Figure 4, comprises head body 36-1, is provided with the toluene liquid-inlet pipe 36-3 that is communicated with toluene feed mouth 15 on head body 36-2 top, and toluene liquid-inlet pipe 36-1 is communicated with toluene film forming chamber 36-5; Described toluene film forming chamber 36-5 is cylindric; On the sidewall of head body 36-2, be provided with the 2-mercapto benzothiazole liquid-inlet pipe 36-1 that is communicated with 2-mercapto benzothiazole opening for feed 14; 2-mercapto benzothiazole liquid-inlet pipe 36-1 is communicated with 2-mercapto benzothiazole film forming chamber 36-4, and described 2-mercapto benzothiazole film forming chamber 36-4 is cylindric; Toluene liquid film forming chamber 36-5 bottom is connected with 2-mercapto benzothiazole film forming chamber 36-4 bottom, and described toluene film forming chamber 36-5 bottom is a conically shaped with the place of being connected, 2-mercapto benzothiazole film forming chamber 36-4 bottom; Head body 36-2 bottom is provided with mixture export 36-7.
Described drying machine is as shown in Figure 5; Comprise dry chamber 46, dry chamber 46 tops are provided with opening for feed 41 and vacuum orifice 52, and the bottom is provided with discharge port 47; Be provided with stir shaft 43 and agitating vane 44 in the dry chamber 46 by drive power source; It is characterized in that: described stir shaft is hollow stir shaft, and the top is provided with steam inlet 50 and vapour outlet 51, and said agitating vane 44 is spiral double-deck agitating vane; The two-layer inner chamber of agitating vane is connected with steam inlet 50 and vapour outlet 51 respectively, and two-layer agitating vane bottom links; Be provided with interlayer 45 at the drying chamber chamber outer wall, interlayer 45 is provided with inlet mouth 48 and air outlet 49.
Described high pressure synthesis system 1 is as shown in Figure 1; Comprise high pressure synthesis reactor 17; Aniline storage tank 15 is connected with high pressure synthesis reactor 17 through aniline test tank 16; Dithiocarbonic anhydride storage tank 11 is connected with sulfur melting kettle 12, and sulfur melting kettle 12 is connected with high pressure synthesis reactor 17 with molten sulphur liquid test tank 14 through dissolving sulphur liquid storage tank 13 successively.
Described exhaust treatment system 3 comprises one-level tourie 18; The vapor pipe of one-level tourie 18 connects dithiocarbonic anhydride holding tank 19; Dithiocarbonic anhydride holding tank 19 bottoms connect dithiocarbonic anhydride storage tank 24; The vapor pipe of dithiocarbonic anhydride holding tank 19 connects secondary tourie 20, three grades of touries 21 and level Four touries 21 successively, and touries at different levels all connect sulphur hydrogen flower sodium storage tank 23.
Operational path of the present invention is following:
1, height is pressed into: with HPP aniline that measures (400 kilograms) and three nitric sulfids (245 kilograms of 400 kilograms+Sulfurs of dithiocarbonic anhydride) are squeezed into the high pressure synthesis reactor successively; Close relevant charging valve on the still; Open the outside electric heater of kettle, feeding temperature-raising.When temperature in the kettle reaches 210 ~ 220 ℃, when pressure reaches 2.0-2.2MPa, closes electric heater, stop to send.When temperature of charge, pressure no longer change in the still, continue to prolong soaking time, when temperature in the kettle drops to 220 ℃, open pressure relief valve, keep relief pipeline internal pressure 0.055-0.06MPa, be zero until the still internal pressure.
2, extraction: open extraction kettle and stir, open toluene valve on the extraction kettle, in autoclave discharging process, continue 2000 liters of toluene of spraying gun adding in extraction kettle.The MBT that dissolves after will synthesizing with 0.03MPa nitrogen is pressed in the extraction kettle spraying gun.Discharging finishes to keep to stir after 15 minutes shuts down; After static 60 minutes stratified supernatant, line strainer is put into mother liquor tank after filtering.Open toluene injection valve on the extraction kettle, in the disposable adding extraction kettle of 1500 liters of toluene that has measured, open extraction kettle and stir, carry out the washing extraction second time, keep stirring and shut down static after 30 minutes.After static 60 minutes stratified supernatant, line strainer is put into mother liquor tank after filtering.Open toluene injection valve on the extraction kettle, in the disposable adding extraction kettle of 1000 liters of toluene that has measured, open extraction kettle and stir; Wash extraction for the third time, keep and stir after 30 minutes, after unlatching extraction kettle bottom dispensing valve is put into mother liquor tank with material; The open vacuum suction filtration; Utilize vacuum that debris is evacuated in the mother liquor tank, when on the suction filtration pipeline, looking domestic no elute, can stop vacuum filtration.
3, drying and crushing and packing: open extraction kettle bottom dispensing valve, three-dimensional drying machine charging valve successively, open the extraction kettle reverse switch, material is depressed in the drying machine.The unlatching drying machine stirs, and opens the drying machine heating unit successively, feeds the 0.04-0.06MPa saturation steam; When built-in temperature is risen to 110 ± 10 ℃; Regulate vacuum tightness to-0.065-0.085MPa, when looking the border on the toluene withdrawing can and not having obvious outflows, shutdown after 30 minutes.Open drying machine bottom dispensing valve, put to charging tray material and pack.Mass transport is pulverized and packed, puts in storage after pulverizing the room.
High pressure synthesis system in the utility model and exhaust treatment system and technology thereof all can adopt prior art.