CN201003039Y - Apparatus for producing benzyl chloride - Google Patents
Apparatus for producing benzyl chloride Download PDFInfo
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- CN201003039Y CN201003039Y CNU2007200346715U CN200720034671U CN201003039Y CN 201003039 Y CN201003039 Y CN 201003039Y CN U2007200346715 U CNU2007200346715 U CN U2007200346715U CN 200720034671 U CN200720034671 U CN 200720034671U CN 201003039 Y CN201003039 Y CN 201003039Y
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Abstract
The utility model provides a benzyl chloride process device, comprising an integrated chlorination tower and a distillation tower. The bottom of the distillation tower is provided with a distillation kettle. The utility model is characterized in that the chlorination tower comprises a chlorination tower segment and a liquid chlorination tower segment; the chlorination tower segment is internally provided with a tube board, an air riser, a liquid down tube with a liquid down cup and a first chloride communicating tube which is communicated with the chloride communicating cut; the lower parts of the air riser and the liquid down tube are tightly fixed on the tube board, and the top of the air riser is higher than that of the liquid down tube; the utility model is also provided with a distillation kettle which is split with the chlorination tower, which is internally provided with a second chloride communicating tube which is communicated with the chloride communicating cut; the utility model is also provided with a condenser and a separating tank, and the condenser is communicated with the chlorination tower, the distillation tower or the distillation kettle through a pipeline. The utility model having the advantages of reasonable structure and safe use, and is capable of restraining ring cleavage reaction in the tower type gas phase chlorination production process of benzyl chloride.
Description
Technical field
The utility model relates to the Benzyl Chloride production equipment of using in a kind of chemical intermediate Benzyl Chloride production.
Background technology
In the prior art, Benzyl Chloride gas (liquid) mutually light chloridization process route to produce employed chlorinated distillation tower be the integral type setting, the chlorination tower is arranged on distillation tower top.During production, in the chlorinated distillation tower, vapor phase toluene and gas phase chlorine reaction utilize reaction---distillation technique, limit coronite distillation, the transformation efficiency that main reaction region control is lower, and the product continuous still battery separates, make the toluene gasification return reaction zone continuously and continue reaction, constantly circulation is finished reaction.The toluene per pass conversion reaches 90%, and the selectivity of Benzyl Chloride reaches 96%.Universities and colleges of domestic a few institute carry on technical development respectively, and about 1997, build nearly ten cover full scale plants at home, the operation of going into operation in succession is because technology is immature, problem is more, wherein, mainly be frequent generation " ring-opening reaction ", i.e. chlorinated distillation tower chlorine port place, the detonation firing accident often takes place, burn the tetrafluoro chlorination card on the chlorine port, downtake, filler etc., even the endoscopy glass in illumination hole goes up, Taka collapses takes off, the displacement of tower joint, the tower pad is washed open, and flame passes in and out in tower, in case out of control, easily cause the fire disaster accident, greatly threaten safety.This detonation ring-opening reaction as shown in the formula:
Here chlorine becomes oxygenant, and between the toluene redox reaction takes place.In liquid phase chlorination technology, this ring-opening reaction occurs in gas-phase space once in a while, and because of multiple reason, excessive chlorine is emitted in the vapor phase toluene, and reach limits of explosion after mixing, detonation taking place, follow sound, flame and high temperature, makes a large amount of toluene open loop charings, generating carbon black is mixed in the material, black in prepared Chinese ink, hydrogen chloride gas that produces during open loop and high temperature make and very easily demolish equipment and pipeline by gas phase partial volume instantaneous expansion several times in the system.
And in existing gas (liquid) phase chloridizing unit, pure toluene vapor at first meets in chlorine that first chlorine port is pure and the distillation tower, mixes, gas-gas-phase reaction takes place, and this is a kind of reaction conditions that is in extreme danger, the temperature of reaction height, bring out this ring-opening reaction easily, and the frequency height, turndown ratio is little.The tetrafluoro chlorination card of chlorine port top is in the position of gas-gas-phase reaction, owing to temperature is out of shape than higher, liquid holdup fluctuation on the card is big, even dried tower, the chlorine maldistribution, assimilation effect is poor, and it is more to go to the chlorine of participating in reaction in the gas-phase space of card top, and ring-opening reaction also takes place easily.So the first layer card is often burnt, must in time change, otherwise will jeopardize second layer card, the 3rd layer of card ... the chain generation of producer's ring-opening reaction that has, 9 layers of card all burn, and loss is serious.Ring-opening reaction is the biggest threat of gas (liquid) phase chlorination safety in production.
In the prior art, it is to adopt gap method chlorination that gas (liquid) phase chlorination process is produced, toluene first distillation and reflux dehydration in still kettle during operation, and then logical chlorine, after chlorination finished, crude product went rectifying still to be steamed into product, still kettle is thrown toluene again and is carried out new round operation, throw toluene, heating, distillation and reflux this several procedures that dewater to still kettle, need to begin chlorination through after 4-5 hour.And after each chlorination finished discharging, still about 180 ℃, if throw new toluene this moment, then still temperature rapid drawdown easily made the sudden and violent porcelain of enamel still damage to the still temperature.Have to still kettle is cooled to 150 ℃ naturally, slowly throw toluene again, the operating time prolongs, and throughput is restricted, and the problem that enamel still damages is still severe.In still formula liquid phase chlorination method production technique, though can adopt continuous processing production, but its raw material toluene could use after all must handling through dewatering unit in advance, thus to set up the distillation type dehydration equipment, so its raw material consumption is relative with production cost also higher.
Summary of the invention
Technical problem to be solved in the utility model is at the deficiencies in the prior art, provide a kind of rational in infrastructure, safe in utilization, can suppress tower gas phase chlorination and produce the Benzyl Chloride production equipment that ring-opening reaction takes place in the Benzyl Chloride process.
Technical problem to be solved in the utility model is to realize by following technical scheme.The utility model is a kind of Benzyl Chloride production equipment, comprises chlorination tower and distillation tower that body-lined type is provided with, and the bottom of distillation tower is provided with still kettle; Be characterized in, the chlorination tower comprises chlorination tower joint and liquid phase chlorination tower joint, liquid phase chlorination Ta Jienei is provided with the downtake of card, riser, band liquid reducing cup and first Chlorination tube that feeds from chlorine port, the bottom of riser and downtake closely is fixed on the card, and the top of riser is higher than the top of downtake; It also is provided with the chlorination tank that is split type setting with the chlorination tower, is provided with second Chlorination tube that feeds from chlorine port in the chlorination tank; It also is provided with condenser and separating tank, and described condenser or separating tank are by pipeline connection chlorination tower, distillation tower or chlorination tank.
Technical problem to be solved by this invention can also further realize by following technical scheme.Above-described device is characterized in, set condenser is 3, i.e. first-stage condenser, secondary condenser and three grades of condensers; Set separating tank is 2, i.e. flash trapping stage jar and secondary separating tank; Described first-stage condenser is communicated with the chlorination top of tower by pipeline; Pass through pipeline connection between first-stage condenser, secondary condenser and three grades of condensers; First-stage condenser, secondary condenser and three grades of condensers are communicated with flash trapping stage jar and secondary separating tank by pipeline respectively; The flash trapping stage jar is communicated with chlorination tank by pipeline; The secondary separating tank is communicated with chlorination tower top by pipeline.
Technical problem to be solved by this invention can also further realize by following technical scheme.Above-described device is characterized in, is connected with the toluene transfer line on the secondary condenser, and the toluene transfer line is provided with the material pump.The toluene that is reclaimed by rectifying still is the same with new toluene, also presses certain continuous injected system of flow by the material pump, participates in continuously dehydrating and continuous chlorination.
Technical problem to be solved by this invention can also further realize by following technical scheme.Above-described device is characterized in, it also is provided with the hydrogenchloride surge tank, and set hydrogenchloride surge tank is communicated with flash trapping stage jar, secondary separating tank and three grades of condensers by pipeline.The volume of separating tank can be selected 500～1000l, and to prolong the residence time of toluene in jar, making wherein, concentrated hydrochloric acid obtains sedimentation fully.Hydrochloric acid in the separating tank will in time enter in the hydrogenchloride surge tank, and regularly the concentrated hydrochloric acid with hydrogenchloride surge tank bottom enters chlorine hydride absorption system concentrated acid circulation tank.
Technical problem to be solved by this invention can also further realize by following technical scheme.Above-described device is characterized in, the external jacket of chlorination tank is provided with vapour line and cooling water pipeline, and is provided with by-pass valve control.This is the temperature for energy double regulation control chlorination tank, improves the Ji Wen of material first at the chlorination initiating stage; Second cooling that can be suitable when chlorination temperature is too high.
Technical problem to be solved by this invention can also further realize by following technical scheme.Above-described device is characterized in, the volume of chlorination tank is 100～300l, and the length of liquid phase chlorination Ta Jienei downtake is 1-1.5 times of tower diameter.This is in order to accelerate the replacing velocity of liquid phase toluene material, to suppress the formation of polychloride.
Technical problem to be solved by this invention can also further realize by following technical scheme.Above-described device is characterized in, the packed height in the distillation tower is 2-3m, and tower diameter is φ 600-800mm.This is in order to improve the crude product separating effect.
Technical problem to be solved by this invention can also further realize by following technical scheme.Above-described device is characterized in, described condenser is 25-30m
2The rectangle graphite condenser.This is in order to reduce the consumption of toluene, to guarantee cooling performance.
Technical problem to be solved by this invention can also further realize by following technical scheme.Above-described device is characterized in, described chlorination tower joint is the 9-11 joint, and tower diameter is φ 600-800mm.This be for the absorption that guarantees chlorine complete.
Technical problem to be solved by this invention can also further realize by following technical scheme.Above-described device is characterized in, is provided with porcelain filling tower joint at the top of chlorination tower; Described liquid phase chlorination tower joint is 1-2, is provided with at interval; Described riser is the 3-5 root; The height of liquid phase chlorination tower joint is 1.5-2.5 times of chlorination tower joint; First Chlorination tube is a 0.4-0.6 rice to the distance at downtake top; The afterbody of described first Chlorination tube and second Chlorination tube is equipped with gas distributor, and second Chlorination tube is inserted into the bottom of chlorination tank.
In order to suppress the generation of impurity such as Benzyl Chloride high temperature self-polymeric reaction and the adjacent chlorine of inhibition, must in still kettle, replenish special assistant continuously in the ratio of toluene feed amount 0.5-1/ ten thousand.
Chlorination tank bottom select suitable upflow tube height can constant chlorination tank in the degree of depth of toluene liquid level, can guarantee that chlorine has long stroke under toluene liquid, improve the assimilation effect of chlorine.
In the entire system operation, regulate and control the heating intensity of still kettle, control total quantity of reflux of toluene, to accelerate chlorination tank and liquid phase chlorination Ta Jienei material replacing velocity, reduce chlorination degree, improve the selectivity of Benzyl Chloride.
If common gases in the chlorination tank is distributed with " a kind of gas distributor " described in the application number 200520140010.1, then also can further suppress the generation of polychloride.
In order to improve light-initiated efficient, on main reaction region chlorination tank and liquid phase chlorination tower joint, 2～3 DN150 illumination holes are set, configuration JLC chromatic metallic halogenide blue-ray light, and be equipped with circular Explosion-proof globe, every lamp power can be selected 175～400W for use, JLC chromatic metallic halogenide blue-ray light of all the other every joint chlorination tower joint illumination hole configurations, and be equipped with circular Explosion-proof globe, every lamp power can be selected 175W for use, and the illumination total power of every chlorination tower configuration is 2～3KW.
The present invention is repeated chlorination for fear of toluene, with chlorination tank and the split type setting of chlorinated distillation tower, in vertical direction, stagger in chlorination tank and chlorinated distillation tower position, the crude product that top liquid phase chlorination tower joint is produced does not flow into chlorination tank, separate and enter distillation tower, then hang oneself the almost approximate pure toluene of first-stage condenser condensation of the material that enters chlorination tank, and the material major part that enters liquid phase chlorination tower joint is hung oneself behind the hydrogen chloride gas drying and dehydrating and abundant settled new toluene, no matter at chlorination tank or liquid phase chlorination Ta Jienei, chlorine only carries out one section chlorination with almost approximate pure liquid phase toluene, does not exist multistage to repeat chlorination.Because of toluene flux big, and this two places reaction vessel volume is little, the material replacing velocity is fast, chlorination degree is low, not only suppress the formation of polychloride effectively, and changed thoroughly that chlorine directly mixes this gas-phase reaction condition that is in extreme danger with the pure toluene steam in the former technology, can suppress the generation of toluene open loop deflagration accident having, to guarantee the Benzyl Chloride safety in production.
The present invention utilizes the hydrogen chloride gas that toluene and chlorine reaction generated in the Benzyl Chloride production process to have the intensive water absorbing properties, continuously raw material toluene is dewatered, the toluene dehydration is carried out synchronously with chlorination, independent thermal dehydration time, facility investment and energy consumption have been saved, realized the chlorination serialization, the toluene continuously feeding, the continuous discharging of Benzyl Chloride crude product, changed the frequent input and output material of former technology enamel still kettle intermittent type, the working condition of the frequent cataclysm of still temperature, not only prolong the work-ing life of enamel still, and improved production efficiency greatly.
Description of drawings
Fig. 1 is a kind of structural representation of the present utility model.
Fig. 2 is the structural representation of liquid phase chlorination tower joint.
Embodiment
Embodiment 1.With reference to Fig. 1, Fig. 2.A kind of Benzyl Chloride production equipment comprises chlorination tower 4 and distillation tower 2 that body-lined type is provided with, and the bottom of distillation tower 2 is provided with still kettle 1; Described chlorination tower 4 comprises chlorination tower joint 6 and liquid phase chlorination tower joint 5, be provided with card 12, riser 13, the downtake 14 of band liquid reducing cup 15 and first Chlorination tube 11 that from chlorine port, feeds in the liquid phase chlorination tower joint 5, the bottom of riser 13 and downtake 14 closely is fixed on the card 12, and the top of riser 13 is higher than the top of downtake 14; It also is provided with the chlorination tank 9 that is split type setting with chlorination tower 4, is provided with second Chlorination tube 10 that feeds from chlorine port in the chlorination tank 9; It also is provided with condenser 16,17, and 18 and separating tank 19,20, described condenser 16,17,18 or separating tank 19,20 are by pipeline connection chlorination tower 4, distillation tower 2 or chlorination tank 9.
Embodiment 2.In embodiment 1 described device, set condenser 16,17,18 is 3, i.e. first-stage condenser 16, secondary condenser 17 and three grades of condensers 18; Set separating tank 19,20 is 2, i.e. flash trapping stage jar 19 and secondary separating tank 20; Described first-stage condenser 16 is communicated with chlorination tower 4 tops by pipeline; Pass through pipeline connection between first-stage condenser 16, secondary condenser 17 and three grades of condensers; First-stage condenser 16, secondary condenser 17 and three grades of condensers 18 are communicated with flash trapping stage jar 19 and secondary separating tank 20 by pipeline respectively; Flash trapping stage jar 19 is communicated with chlorination tank 9 by pipeline; Secondary separating tank 20 is communicated with chlorination tower 4 tops by pipeline.
Embodiment 3.In embodiment 2 described devices, be connected with the toluene transfer line on the secondary condenser 17, the toluene transfer line is provided with material pump 21.
Embodiment 4.In embodiment 2 described devices, it also is provided with hydrogenchloride surge tank 22, and set hydrogenchloride surge tank 22 is communicated with flash trapping stage jar 19, secondary separating tank 20 and three grades of condensers 18 by pipeline.
Embodiment 5.In any one described device, the external jacket of chlorination tank 9 is provided with vapour line and cooling water pipeline in embodiment 1-4, and is provided with by-pass valve control.
Embodiment 6.In any one described device, the volume of chlorination tank 9 is 100l in embodiment 1-4; The length of liquid phase chlorination tower joint 5 interior downtakes 14 is 1 times of tower diameter.
Embodiment 7.In any one described device, the volume of chlorination tank 9 is 300l in embodiment 1-4; The length of liquid phase chlorination tower joint 5 interior downtakes 14 is 1.5 times of tower diameter.
Embodiment 8.In any one described device, the packed height in the distillation tower 2 is 2m in embodiment 1-4, and tower diameter is φ 600mm.
Embodiment 9.In any one described device, the packed height in the distillation tower 2 is 3m in embodiment 1-4, and tower diameter is φ 800mm.
Embodiment 10.In any one described device, described condenser 16,17,18 is 25m in embodiment 1-4
2The rectangle graphite condenser.
Embodiment 11.In any one described device, described condenser 16,17,18 is 30m in embodiment 1-4
2The rectangle graphite condenser.
Embodiment 12.In any one described device, described chlorination tower joint 6 is 9 joints in embodiment 1-4, and tower diameter is φ 600mm.
Embodiment 13.In any one described device, described chlorination tower joint 6 is 11 joints in embodiment 1-4, and tower diameter is φ 800mm.
Embodiment 14.In embodiment 1-4, in any one described device, be provided with porcelain filling tower joint 7 at the top of chlorination tower 4; Described liquid phase chlorination tower joint 5 is 1, and described riser 13 is 3; The height of liquid phase chlorination tower joint 5 is 1.5 times of chlorination tower joint 6; First Chlorination tube 11 is 0.4 meter to the distance at downtake 14 tops; The afterbody of described first Chlorination tube 11 and second Chlorination tube 10 is equipped with gas distributor, and second Chlorination tube 10 is inserted into the bottom of chlorination tank 9.
Embodiment 15.In embodiment 1-4, in any one described device, be provided with porcelain filling tower joint 7 at the top of chlorination tower 4; Described liquid phase chlorination tower joint 5 is 2, is provided with at interval; Described riser 13 is 5; The height of liquid phase chlorination tower joint 5 is 2.5 times of chlorination tower joint 6; First Chlorination tube 11 is 0.6 meter to the distance at downtake 14 tops; The afterbody of described first Chlorination tube 11 and second Chlorination tube 10 is equipped with gas distributor, and second Chlorination tube 10 is inserted into the bottom of chlorination tank 9.
Embodiment 16.With reference to Fig. 1, Fig. 2.A kind of Benzyl Chloride production equipment comprises chlorination tower 4 and distillation tower 2 that body-lined type is provided with, and the bottom of distillation tower 2 is provided with still kettle 1; Described chlorination tower 4 comprises chlorination tower joint 6 and liquid phase chlorination tower joint 5, be provided with card 12, riser 13, the downtake 14 of band liquid reducing cup 15 and first Chlorination tube 11 that from chlorine port, feeds in the liquid phase chlorination tower joint 5, the bottom of riser 13 and downtake 14 closely is fixed on the card 12, and the top of riser 13 is higher than the top of downtake 14; It also is provided with the chlorination tank 9 that is split type setting with chlorination tower 4, is provided with second Chlorination tube 10 that feeds from chlorine port in the chlorination tank 9; It also is provided with condenser 16,17, and 18 and separating tank 19,20, described condenser 16,17,18 or separating tank 19,20 are by pipeline connection chlorination tower 4, distillation tower 2 or chlorination tank 9.
Be connected with the toluene transfer line on the secondary condenser 17, the toluene transfer line is provided with material pump 21.
It also is provided with hydrogenchloride surge tank 22, and set hydrogenchloride surge tank 22 is communicated with flash trapping stage jar 19, secondary separating tank 20 and three grades of condensers 18 by pipeline.
The external jacket of chlorination tank 9 is provided with vapour line and cooling water pipeline, and is provided with by-pass valve control.
The volume of chlorination tank 9 is 2001; The length of liquid phase chlorination tower joint 5 interior downtakes 14 is 1.2 times of tower diameter.
Packed height in the distillation tower 2 is 2.5m, and tower diameter is φ 800mm.
Described condenser 16,17,18 is 30m
2The rectangle graphite condenser.
Described chlorination tower joint 6 is 10 joints, and tower diameter is φ 800mm.
The driving initial stage, new toluene of raw material and auxiliary agent are dropped into intensification in the still kettle 1, because of toluene and water azeotropic, toluene steam and water vapor are through distillation tower 2, chlorination tower 4 enters in the first-stage condenser 16, through condensation, toluene imports separating tank 19 bottoms together with water, heavy moisture then is deposited in the bottom of separating tank 19, and the toluene of light specific gravity flows into chlorination tank 9 through separating tank 19 top overflow ports, the water yield of the recirculated cooling water of regulation and control condenser 16, make the toluene temperature that flows into chlorination tank 9 satisfy toluene and be initiated the chlorating starting temperature, after toluene amasss and expires in the chlorination tank 9, just enter distillation tower 2 automatically through the bottom upflow tube, then turn back to still kettle 1, in still kettle 1, reheated again, with residual water-content azeotropic in the toluene, reevaporate, so constantly toluene moisture content has been taken off in circulation.In dehydration, the heating intensity of regulation and control still kettle 1 keeps certain toluene evaporates amount, could keep enough liquid height of holding on each layer chlorination card.
Slowly open chlorination tank 9 logical chlorine valve doors, chlorine enters chlorination tank 9 through second Chlorination tube 10, through light-initiated, chlorine is chlorine atom and toluene reaction by homolysis, accelerate logical chlorine speed gradually, Benzyl Chloride crude product that generates and unreacted toluene import distillation tower 2 by chlorination tank 9 bottom upflow tubes, liquid distributor 3 and filler mass transfer separate in tower, the product Benzyl Chloride enters still kettle 1, and being distilled the still heating evaporation, unreacted toluene rises to chlorination tower 4, with gas---the toluene steam that comes by reacting heat evaporation in the chlorination tank 9 upper gaseous phase pipelines importing tower, hydrogen chloride gas that reaction generates and remaining chlorine---mix, carry out respectively in the above and below of chlorination tower 4 each layer of Lower Half chlorination cards solution-air gentle-gas-phase reaction, remaining chlorine is absorbed fully.Because most chlorine of second Chlorination tube 10 are fully reacted away under chlorination tank 9 toluene liquid, a small amount of unreacted chlorine of overflowing equals to be diluted by a large amount of hydrogenchloride, so gas-gas-phase reaction that the card below is taken place is gentle, heat release is not remarkable, card is indeformable, so just can suppress the generation of first Chlorination tube place toluene open loop deflagration accident having.
Slowly open the second logical chlorine valve door again, make chlorine enter liquid phase chlorination tower joint 5 through first Chlorination tube 11, behind Photoinitiated reactions, accelerate logical chlorine speed gradually, the crude product that generates not on the cracked ends card 12 downtake 14 and liquid reducing cup 15 successively flow into lower floor's chlorination card, separate through distillation tower 2, Benzyl Chloride operation downwards enters still kettle 1, unreacted toluene is constantly upwards moved by gasification under the dual function of reaction heat and still kettle 1 heating, successively enter each layer chlorination card, and carry out solution-air and gas-gas-phase reaction respectively in the above and below of chlorination card, chlorine is absorbed fully.As a same reason, most chlorine of first Chlorination tube 11 are fully absorbed under the toluene liquid in liquid phase chlorination tower joint 5, overflow a small amount of unreacted chlorine because of being diluted by a large amount of hydrogenchloride, so, gas-the gas-phase reaction of carrying out below chlorination tower 4 first half chlorination cards also is gentle, heat release is not remarkable, and card is indeformable, so just can suppress the generation of the first Chlorination tube 11 places toluene open loop deflagration accident having.
Hydrogen chloride gas that chlorination reaction produces and absorption reaction heat and the toluene steam of evaporation mix and enter 16 step by step, 17,18 condensers are cooled, most of toluene steam is condensed in condenser 16, and by inserting tube importing separating tank 19 bottoms, in separating tank 19, obtain sufficient sedimentation, be deposited on separating tank 19 bottoms, the toluene that proportion is lighter then flows in the chlorination tanks 9 from separating tank 19 top overflow ports and reacts with chlorine wherein heavy concentrated hydrochloric acid---these concentrated hydrochloric acids by the moisture absorption of carrying secretly in moisture remaining in the toluene and the chlorine hydrogenchloride form---.The uncooled toluene steam of another small portion is chlorinated hydrogen and carries secretly and enter in the condenser 17, by condensation once more, and by inserting tube importing separating tank 20 bottoms, in separating tank 20, obtain abundant sedimentation, with the wherein heavy concentrated hydrochloric acid of sedimentation, the lighter toluene of proportion, continues and chlorine reaction in top of tower turns back to chlorination tower 4 then from separating tank 20 top overflow ports.The toluene steam of minute quantity is chlorinated hydrogen and carries secretly and enter in the condenser 18, because of condenser 18 adopts the chilled brines cooling, thereby makes toluene obtain sufficient condensation, and imports separating tank 20 bottoms by inserting tube.The hydrogen chloride gas of discharging from condenser 18 then passes through hydrogenchloride surge tank 22, delivers to chlorine hydride absorption system again, absorbs through water to make by-product hydrochloric acid.
Along with chlorination is constantly carried out, the toluene component constantly reduces in the still kettle 1, and the Benzyl Chloride component constantly increases, then still kettle 1 still temperature continues to rise, when the still temperature reaches 175～180 ℃, expression has obtained the Benzyl Chloride crude product of high conversion in the still, then can change over to advance new toluene, continuously dehydrating, continuous chlorination continuously, go out the operation of crude product continuously.Start toluene material pump 21 this moment, to inject condenser 17 inlet mouths by certain flow through the new toluene of nature standing sedimentation more than 48 hours, liquid distributor disperses in inlet mouth, make the toluene vertical hole of graphite block inwall in condenser 17 form falling liquid film, fully contact with the hydrogen chloride gas following current, moisture content in the toluene generates concentrated hydrochloric acid because of absorbing hydrogen chloride, import separating tank 20 bottoms together with condensation toluene by inserting tube, heavy concentrated hydrochloric acid is deposited on separating tank 20 bottoms, the toluene of light specific gravity then enters chlorination tower 4 from separating tank 20 top overflow ports through the top, separate by the filler mass transfers that liquid distributor in the tower 8 distributes with tower saves in 7, moisture remaining in the toluene is evaporated then, and be mixed into condenser 16 with hydrogen chloride gas and toluene vapor and be condensed, import separating tank 19 bottoms by inserting tube, remaining moisture is deposited on separating tank 19 bottoms because of absorbing hydrogen chloride gas generates heavy concentrated hydrochloric acid, and the toluene of light specific gravity then flows into chlorination tank 9 from separating tank 19 top overflow ports and participates in chlorination reaction.
Because of the continuous input of new toluene and chlorine, material liquid surface then continues to rise in the still kettle 1, utilizes potential difference, crude product voluntarily continuous overflow to the crude product basin, will install by-pass valve control additional on overflow passage, control crude product flooding velocity is with the liquid level in the constant still kettle 1.Also can crude product directly be evacuated to rectifying still continuously by the constant flow carry out rectifying without the crude product jar.
Claims (10)
1, a kind of Benzyl Chloride production equipment comprises chlorination tower (4) and distillation tower (2) that body-lined type is provided with, and the bottom of distillation tower (2) is provided with still kettle (1); It is characterized in that, described chlorination tower (4) comprises chlorination tower joint (6) and liquid phase chlorination tower joint (5), be provided with card (12), riser (13), the downtake (14) of band liquid reducing cup (15) and first Chlorination tube (11) that from chlorine port, feeds in the liquid phase chlorination tower joint (5), the bottom of riser (13) and downtake (14) closely is fixed on the card (12), and the top of riser (13) is higher than the top of downtake (14); It also is provided with the chlorination tank (9) that is split type setting with chlorination tower (4), is provided with second Chlorination tube (10) that feeds from chlorine port in the chlorination tank (9); It also is provided with condenser (16,17,18) and separating tank (19,20), and described condenser (16,17,18) or separating tank (19,20) are by pipeline connection chlorination tower (4), distillation tower (2) or chlorination tank (9).
2, device according to claim 1 is characterized in that, set condenser (16,17,18) is 3, i.e. first-stage condenser (16), secondary condenser (17) and three grades of condensers (18); Set separating tank (19,20) is 2, i.e. flash trapping stage jar (19) and secondary separating tank (20); Described first-stage condenser (16) is communicated with chlorination tower (4) top by pipeline; Pass through pipeline connection between first-stage condenser (16), secondary condenser (17) and three grades of condensers; First-stage condenser (16), secondary condenser (17) and three grades of condensers (18) are communicated with flash trapping stage jar (19) and secondary separating tank (20) by pipeline respectively; Flash trapping stage jar (19) is communicated with chlorination tank (9) by pipeline; Secondary separating tank (20) is communicated with chlorination tower (4) top by pipeline.
3, device according to claim 2 is characterized in that, secondary condenser is connected with the toluene transfer line on (17), and the toluene transfer line is provided with material pump (21).
4, device according to claim 2 is characterized in that, it also is provided with hydrogenchloride surge tank (22), and set hydrogenchloride surge tank (22) is communicated with flash trapping stage jar (19), secondary separating tank (20) and three grades of condensers (18) by pipeline.
According to any one described device among the claim 1-4, it is characterized in that 5, the external jacket of chlorination tank (9) is provided with vapour line and cooling water pipeline, and is provided with by-pass valve control.
According to any one described device among the claim 1-4, it is characterized in that 6, the volume of chlorination tank (9) is 100～300l; The length of liquid phase chlorination tower joint (5) interior downtake (14) is 1-1.5 times of tower diameter.
According to any one described device among the claim 1-4, it is characterized in that 7, the packed height in the distillation tower (2) is 2-3m, tower diameter is φ 600-800mm.
According to any one described device among the claim 1-4, it is characterized in that 8, described condenser (16,17,18) is 25-30m
2The rectangle graphite condenser.
According to any one described device among the claim 1-4, it is characterized in that 9, described chlorination tower joint (6) is the 9-11 joint, tower diameter is φ 600-800mm.
10, according to any one described device among the claim 1-4, it is characterized in that, be provided with porcelain filling tower joint (7) at the top of chlorination tower (4); Described liquid phase chlorination tower joint (5) is 1-2, is provided with at interval; Described riser (13) is the 3-5 root; The height of liquid phase chlorination tower joint (5) is 1.5-2.5 times of chlorination tower joint (6); First Chlorination tube (11) is a 0.4-0.6 rice to the distance at downtake (14) top; The afterbody of described first Chlorination tube (11) and second Chlorination tube (10) is equipped with gas distributor, and second Chlorination tube (10) is inserted into the bottom of chlorination tank (9).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNU2007200346715U CN201003039Y (en) | 2007-02-10 | 2007-02-10 | Apparatus for producing benzyl chloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNU2007200346715U CN201003039Y (en) | 2007-02-10 | 2007-02-10 | Apparatus for producing benzyl chloride |
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| CN201003039Y true CN201003039Y (en) | 2008-01-09 |
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| CNU2007200346715U Expired - Fee Related CN201003039Y (en) | 2007-02-10 | 2007-02-10 | Apparatus for producing benzyl chloride |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101250085B (en) * | 2008-03-13 | 2010-05-26 | 山东聊城中盛蓝瑞化工有限公司 | Benzyl chloride continuous chlorination production technology |
| CN102278868A (en) * | 2011-08-02 | 2011-12-14 | 济南圣泉集团股份有限公司 | Exhaust gas recycling technology and device in isothiocyanate preparation |
| CN104841341A (en) * | 2015-05-25 | 2015-08-19 | 南通江山农药化工股份有限公司 | Outer-tower downcomer chlorination tower and running process thereof |
| CN113173831A (en) * | 2021-04-08 | 2021-07-27 | 宜都市友源实业有限公司 | Production system and process for continuous chlorination of trichlorotoluene |
-
2007
- 2007-02-10 CN CNU2007200346715U patent/CN201003039Y/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101250085B (en) * | 2008-03-13 | 2010-05-26 | 山东聊城中盛蓝瑞化工有限公司 | Benzyl chloride continuous chlorination production technology |
| CN102278868A (en) * | 2011-08-02 | 2011-12-14 | 济南圣泉集团股份有限公司 | Exhaust gas recycling technology and device in isothiocyanate preparation |
| CN104841341A (en) * | 2015-05-25 | 2015-08-19 | 南通江山农药化工股份有限公司 | Outer-tower downcomer chlorination tower and running process thereof |
| CN113173831A (en) * | 2021-04-08 | 2021-07-27 | 宜都市友源实业有限公司 | Production system and process for continuous chlorination of trichlorotoluene |
| CN113173831B (en) * | 2021-04-08 | 2024-01-19 | 宜都市友源实业有限公司 | Production system and process for continuous chlorination of trichlorotoluene |
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