CN2844120Y - Chlorinated distillating tower - Google Patents

Chlorinated distillating tower Download PDF

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Publication number
CN2844120Y
CN2844120Y CN 200520140008 CN200520140008U CN2844120Y CN 2844120 Y CN2844120 Y CN 2844120Y CN 200520140008 CN200520140008 CN 200520140008 CN 200520140008 U CN200520140008 U CN 200520140008U CN 2844120 Y CN2844120 Y CN 2844120Y
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chlorination
tower
chlorine
distillation tower
liquid phase
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CN 200520140008
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张国胜
张华民
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Abstract

The utility model relates to a chlorination distillation tower, which comprises a chlorination tower and a distillation tower. The utility model is characterized in that the chlorination tower and the distillation tower are arranged in a separate arrangement mode, and the chlorination tower and the distillation tower are connected with each other by pipe passages; the chlorination tower comprises a chlorination tower section, a chlorination kettle and a liquid phase chlorine passing tower section; the chlorination kettle is arranged on the bottom of the chlorination tower; a first chlorine passing pipe led into from a chlorine passing mouth is arranged in the chlorination kettle; a pattern board, an air rising pipe, a liquid falling pipe with a liquid falling cup, and a second chlorine passing pipe led into from the chlorine passing mouth are arranged in the liquid phase chlorine passing tower section; the lower part of the air rising pipe and the liquid falling pipe are tightly fixed on the pattern board; the top end of the air rising pipe is higher than the top end of the liquid falling pipe. The utility model has the advantage of simple structure and can effectively inhibit the occurrence of ring opening accidents to ensure the safe production of benzyl chloride.

Description

A kind of chlorinated distillation tower
Technical field
The utility model relates to the chlorinated distillation tower of using in a kind of chemical intermediate Benzyl Chloride production.
Background technology
In the prior art, the chlorinated distillation tower that gas phase light chloridization process route uses when producing Benzyl Chloride is the integral type setting, and the chlorination tower is arranged on the top of distillation tower.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 constantly return reaction zone 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, go into operation in succession and move, but expose many problems, mainly be frequent generation " ring-opening reaction ", promptly the detonation firing accident often takes place in chlorinated distillation tower chlorine port place, the tetrafluoro that burns on the chlorine port leads to chlorine card, downtake, filler etc., even the endoscopy glass in illumination hole demolition, Taka collapses takes off, and the tower pad is washed open, 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:
Figure Y20052014000800041
Here chlorine serves as oxygenant, and between the toluene redox reaction takes place.In liquid phase chlorination, this ring-opening reaction occurs in gas-phase space once in a while.Because of multiple reason, excessive chlorine is emitted in the vapor phase toluene, and reach limits of explosion after mixing, and detonation takes place, follow sound, flame and high temperature, make a large amount of toluene open loop charings, the carbon black that generates is mixed in the material, and is black in prepared Chinese ink, because the hydrogenchloride of high temperature and formation, gas phase partial volume instantaneous expansion several times very easily demolish equipment and pipeline in the system.
And in the gas phase chlorination device, pure toluene vapor at first meets in chlorine that first chlorine port is pure and the distillation tower, mixes, and gas-gas-phase reaction takes place, and the temperature of reaction height brings out this ring-opening reaction easily, and the frequency height, and turndown ratio is little.The logical chlorine card of the tetrafluoro of chlorine port top is in the position of gas-gas-phase reaction, owing to temperature is out of shape than higher, the fluid wave of holding on the card moves 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 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 phase chlorination safety in production.
Summary of the invention
Technical problem to be solved in the utility model is at the deficiencies in the prior art, provides a kind of and can suppress the chlorinated distillation tower that tower gas phase chlorination is produced generation ring-opening reaction 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 chlorinated distillation tower, comprises chlorination tower and distillation tower, is characterized in, described chlorination tower and distillation tower adopt split type setting, and connect by pipeline between the two; The chlorination tower comprises the logical chlorine tower joint of chlorination tower joint, chlorination tank and liquid phase; Chlorination tank is located at the chlorination tower bottom, be provided with first Chlorination tube that from chlorine port, feeds in the chlorination tank, the logical chlorine Ta Jienei of liquid phase is provided with the downtake of card, riser, band liquid reducing cup and second 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.
Technical problem to be solved in the utility model can also further realize by following technical scheme.Above-described a kind of chlorinated distillation tower is characterized in, second Chlorination tube is horizontally placed on the middle and lower part of the logical chlorine tower joint of liquid phase.
Technical problem to be solved in the utility model can also further realize by following technical scheme.Above-described a kind of chlorinated distillation tower is characterized in, is provided with porcelain filling tower joint at the top of chlorination tower.
Technical problem to be solved in the utility model can also further realize by following technical scheme.Above-described a kind of chlorinated distillation tower is characterized in, the logical chlorine tower joint of described liquid phase is 1-2, is provided with at interval.The number of the logical chlorine tower joint of the liquid phase that the utility model was provided with can be selected to be provided with in the production application process as required.
Technical problem to be solved in the utility model can also further realize by following technical scheme.Above-described a kind of chlorinated distillation tower is characterized in that described riser is the 3-5 root.The radical of the riser that the utility model was provided with also can be selected to be provided with in the production application process as required.Be generally even setting.
Technical problem to be solved in the utility model can also further realize by following technical scheme.Above-described a kind of chlorinated distillation tower is characterized in, the height of the logical chlorine tower joint of liquid phase is 1.5-2.5 times of chlorination tower joint.Like this, can guarantee effectively that this tower saves the height of holding liquid, suppresses the generation of open loop accident.
Technical problem to be solved in the utility model can also further realize by following technical scheme.Above-described a kind of chlorinated distillation tower is characterized in, second Chlorination tube is a 0.4-0.6 rice to the distance at downtake top.Like this, can guarantee effectively that also Chlorination tube inserts the degree of depth in the liquid phase toluene, suppresses the generation of open loop accident.
Technical problem to be solved in the utility model can also further realize by following technical scheme.Above-described a kind of chlorinated distillation tower is characterized in, the pipeline that connects between chlorination tower, the distillation tower is gas phase pipe and liquid phase upflow tube, all adopts enamel or inner liner polytetrafluoroethylene material conduit.
Technical problem to be solved in the utility model can also further realize by following technical scheme.Above-described a kind of chlorinated distillation tower is characterized in that the afterbody of described first Chlorination tube and second Chlorination tube is equipped with gas distributor, and first Chlorination tube is inserted into the bottom of chlorination tank.Like this, can further promote to react evenly, carry out smoothly.
By application of the present utility model, in essence the original easily gas-solid/liquid/gas reactions at open loop position is changed into gas-liquid reaction.Specifically, exactly the chlorinated distillation tower that was integrated originally, be divided into separately independently distillation tower and two parts of chlorination tower, the chlorination tank that is provided with (the little enamel kettle about an available 100-300L) is as chlorination tower coxopodite.Toluene becomes steam condition at the still kettle ebuillition of heated, rise, through distillation tower, enter the chlorination tower, after become liquid phase toluene through condenser cooling and get back to the chlorination tower, get back in the chlorination tank through each downtake, the chlorination tank material liquid surface is got back to distillation tower from overflow spout after reaching certain altitude voluntarily, in porcelain ring surface vapour-liquid counter current contact, carry out mass transfer and heat transfer, reach and balance each other.Chlorination tank is a main reaction region, chlorine is distributed in the liquid phase toluene through first Chlorination tube, carry out gas-liquid phase reaction, the chlorine of the overwhelming majority fully reacts away under toluene liquid, generate Benzyl Chloride and HCl, the HCl gas of a small amount of unreacted chlorine and generation mixes overflows, and the toluene steam of coming with the distillation tower evaporation mixes once again, and above each logical chlorine card of chlorination tower lower part, finish gas-liquid phase reaction, gas-gas-phase reaction is finished in the below.A small amount of unreacted chlorine equals to have been diluted by a large amount of HCl, and such gas-gas-phase reaction, gas-liquid phase reaction are gentle, and heat release is not remarkable, can suppress the generation of ring-opening reaction accident.In this main reaction region of chlorination tank, reaction heat is absorbed by liquid phase toluene, and the toluene temperature rises, if surpass toluene boiling point (110 ℃) temperature, then toluene will be gasified in the chlorination tank, and the toluene liquid level will descend in the still, and the chlorine stroke shortens and the chlorine effect is eaten in influence.So, suitably open chlorination tank chuck water coolant summer, remove the reaction heat of main reaction region, keep little still temperature to equal or a little more than the toluene boiling point, then toluene is in liquefaction all the time, just can keep the liquid level of toluene in the chlorination tank, then the stroke of chlorine is long, has guaranteed the chlorine assimilation effect.
The logical chlorine tower joint of liquid phase of the present utility model can directly process, also can on the basis of former chlorination tower joint, improve, during improvement, logical chlorine card between two chlorination tower joints is removed, and the logical chlorine card of its underpart is replaced by the card (card itself does not have chlorine flow opening) of band riser and downtake, thereby make two chlorination towers joints change the logical chlorine tower joint of liquid phase of the present utility model into.The utility model can be controlled liquid and be raised, second Chlorination tube is inserted into holds in the liquid, major part is absorbed under the liquid holding to make chlorine, remaining chlorine continues to carry out gas-liquid, gas-gas-phase reaction respectively at each logical chlorine card upper and lower of the chlorination tower first half after by a large amount of HCl gas dilutions, thereby make reaction become gentle, suppress the generation of ring-opening reaction accident.
Because the boiling point height of Benzyl Chloride, the Benzyl Chloride that generates at each logical chlorine card upper and lower of the chlorination tower liquefaction of condensing, move down, finally enter still kettle, unreacted toluene is reheated in still kettle, and evaporation moves up, mass-and heat-transfer turns back to reaction zone through distillation tower internal ceramic ring surface, continue and chlorine reaction, go round and begin again, finish reaction.Owing in the whole chlorination reaction,, and then improve the material replacing velocity by the total quantity of reflux of control toluene and the volume of chlorination tank, reduce chlorination degree, then can not influence the selectivity of Benzyl Chloride.In order to improve efficiency of initiation, on the joint of the tower on the little still of main reaction region, 2-3 DN150 illumination hole is set, configuration CJD blue non-ferrous metal halide lamp of series and round lampshade, every lamp power can be selected 175-400W, save the power of all the other illumination hole lamps at each tower and can select several 175W lamps, total illumination power of every chlorination tower configuration is about 2000W.
Compared with prior art, the utility model is simple in structure, can suppress the generation of open loop accident effectively, to guarantee the Benzyl Chloride safety in production.
Description of drawings
Fig. 1 is a kind of structural representation of the present utility model.
Fig. 2 is the partial enlarged drawing of Fig. 1.
Embodiment
Embodiment 1.With reference to Fig. 1, Fig. 2.A kind of chlorinated distillation tower comprises chlorination tower 2 and distillation tower 1, and described chlorination tower 2 and distillation tower 1 adopt split type setting, and connect by pipeline between the two; Chlorination tower 2 comprises the logical chlorine tower joint 3 of chlorination tower joint 4, chlorination tank 6 and liquid phase; Chlorination tank 6 is located at chlorination tower 2 bottoms, be provided with first Chlorination tube 7 that from chlorine port, feeds in the chlorination tank 6, be provided with card 9, riser 12, the downtake 11 of band liquid reducing cup 8 and second Chlorination tube 10 that from chlorine port, feeds in the logical chlorine tower joint 3 of liquid phase, the bottom of riser 12 and downtake 11 closely is fixed on the card 9, and the top of riser 12 is higher than the top of downtake 11.
Embodiment 2.With reference to Fig. 1, Fig. 2.A kind of chlorinated distillation tower comprises chlorination tower 2 and distillation tower 1, and described chlorination tower 2 and distillation tower 1 adopt split type setting, and connect by pipeline between the two; Chlorination tower 2 comprises the logical chlorine tower joint 3 of chlorination tower joint 4, chlorination tank 6 and liquid phase; Chlorination tank 6 is located at chlorination tower 2 bottoms, be provided with first Chlorination tube 7 that from chlorine port, feeds in the chlorination tank 6, be provided with card 9, riser 12, the downtake 11 of band liquid reducing cup 8 and second Chlorination tube 10 that from chlorine port, feeds in the logical chlorine tower joint 3 of liquid phase, the bottom of riser 12 and downtake 11 closely is fixed on the card 9, and the top of riser 12 is higher than the top of downtake 11; Second Chlorination tube 10 is horizontally placed on the middle and lower part of the logical chlorine tower joint 3 of liquid phase; Be provided with porcelain filling tower joint 5 at the top of chlorination tower 2; The pipeline that connects between chlorination tower 2, the distillation tower 1 is gas phase pipe and liquid phase upflow tube, all adopts enamel or inner liner polytetrafluoroethylene material conduit; The afterbody of described first Chlorination tube 7 and second Chlorination tube 10 is equipped with gas distributor, and first Chlorination tube 7 is inserted into the bottom of chlorination tank 6.
Embodiment 3.With reference to Fig. 1, Fig. 2.A kind of chlorinated distillation tower comprises chlorination tower 2 and distillation tower 1, and described chlorination tower 2 and distillation tower 1 adopt split type setting, and connect by pipeline between the two; Chlorination tower 2 comprises the logical chlorine tower joint 3 of chlorination tower joint 4, chlorination tank 6 and liquid phase; Chlorination tank 6 is located at chlorination tower 2 bottoms, be provided with first Chlorination tube 7 that from chlorine port, feeds in the chlorination tank 6, be provided with card 9, riser 12, the downtake 11 of band liquid reducing cup 8 and second Chlorination tube 10 that from chlorine port, feeds in the logical chlorine tower joint 3 of liquid phase, the bottom of riser 12 and downtake 11 closely is fixed on the card 9, and the top of riser 12 is higher than the top of downtake 11; Second Chlorination tube 10 is horizontally placed on the middle and lower part of the logical chlorine tower joint 3 of liquid phase; Be provided with porcelain filling tower joint 5 at the top of chlorination tower 2; The logical chlorine tower joint 3 of described liquid phase is 2, is provided with at interval; Described riser 12 is 5; The height of the logical chlorine tower joint 3 of liquid phase is 1.5 times of chlorination tower joint 4; Second Chlorination tube 10 is 0.4 meter to the distance at downtake 11 tops; The pipeline that connects between chlorination tower 2, the distillation tower 1 is gas phase pipe and liquid phase upflow tube, all adopts enamel or inner liner polytetrafluoroethylene material conduit; The afterbody of described first Chlorination tube 7 and second Chlorination tube 10 is equipped with gas distributor, and first Chlorination tube 7 is inserted into the bottom of chlorination tank 6.
Embodiment 4.With reference to Fig. 1, Fig. 2.A kind of chlorinated distillation tower comprises chlorination tower 2 and distillation tower 1, and described chlorination tower 2 and distillation tower 1 adopt split type setting, and connect by pipeline between the two; Chlorination tower 2 comprises the logical chlorine tower joint 3 of chlorination tower joint 4, chlorination tank 6 and liquid phase; Chlorination tank 6 is located at chlorination tower 2 bottoms, be provided with first Chlorination tube 7 that from chlorine port, feeds in the chlorination tank 6, be provided with card 9, riser 12, the downtake 11 of band liquid reducing cup 8 and second Chlorination tube 10 that from chlorine port, feeds in the logical chlorine tower joint 3 of liquid phase, the bottom of riser 12 and downtake 11 closely is fixed on the card 9, and the top of riser 12 is higher than the top of downtake 11; Second Chlorination tube 10 is horizontally placed on the middle and lower part of the logical chlorine tower joint 3 of liquid phase; Be provided with porcelain filling tower joint 5 at the top of chlorination tower 2; The logical chlorine tower joint 3 of described liquid phase is 1; Described riser 12 is 4; The height of the logical chlorine tower joint 3 of liquid phase is 2 times of chlorination tower joint 4; Second Chlorination tube 10 is 0.5 meter to the distance at downtake 11 tops; The pipeline that connects between chlorination tower 2, the distillation tower 1 is gas phase pipe and liquid phase upflow tube, all adopts enamel or inner liner polytetrafluoroethylene material conduit; The afterbody of described first Chlorination tube 7 and second Chlorination tube 10 is equipped with gas distributor, and first Chlorination tube 7 is inserted into the bottom of chlorination tank 6.
Embodiment 5.With reference to Fig. 1, Fig. 2.A kind of chlorinated distillation tower comprises chlorination tower 2 and distillation tower 1, and described chlorination tower 2 and distillation tower 1 adopt split type setting, and connect by pipeline between the two; Chlorination tower 2 comprises the logical chlorine tower joint 3 of chlorination tower joint 4, chlorination tank 6 and liquid phase; Chlorination tank 6 is located at chlorination tower 2 bottoms, be provided with first Chlorination tube 7 that from chlorine port, feeds in the chlorination tank 6, be provided with card 9, riser 12, the downtake 11 of band liquid reducing cup 8 and second Chlorination tube 10 that from chlorine port, feeds in the logical chlorine tower joint 3 of liquid phase, the bottom of riser 12 and downtake 11 closely is fixed on the card 9, and the top of riser 12 is higher than the top of downtake 11; Second Chlorination tube 10 is horizontally placed on the middle and lower part of the logical chlorine tower joint 3 of liquid phase; Be provided with porcelain filling tower joint 5 at the top of chlorination tower 2; The logical chlorine tower joint 3 of described liquid phase is 1; Described riser 12 is 3; The height of the logical chlorine tower joint 3 of liquid phase is 2.5 times of chlorination tower joint 4; Second Chlorination tube 10 is 0.6 meter to the distance at downtake 11 tops.

Claims (9)

1, a kind of chlorinated distillation tower comprises chlorination tower (2) and distillation tower (1), it is characterized in that, described chlorination tower (2) and distillation tower (1) adopt split type setting, and connect by pipeline between the two; Chlorination tower (2) comprises the logical chlorine tower joint of chlorination tower joint (4), chlorination tank (6) and liquid phase (3); Chlorination tank (6) is located at chlorination tower (2) bottom, be provided with first Chlorination tube (7) that from chlorine port, feeds in the chlorination tank (6), be provided with card (9), riser (12), the downtake (11) of band liquid reducing cup (8) and second Chlorination tube (10) that from chlorine port, feeds in the logical chlorine tower joint of liquid phase (3), the bottom of riser (12) and downtake (11) closely is fixed on the card (9), and the top of riser (12) is higher than the top of downtake (11).
2, a kind of chlorinated distillation tower according to claim 1 is characterized in that, second Chlorination tube (10) is horizontally placed on the middle and lower part of the logical chlorine tower joint of liquid phase (3).
3, a kind of chlorinated distillation tower according to claim 1 is characterized in that, is provided with porcelain filling tower joint (5) at the top of chlorination tower (2).
4, a kind of chlorinated distillation tower according to claim 1 is characterized in that, the logical chlorine tower joint of described liquid phase (3) is 1-2, is provided with at interval.
5, a kind of chlorinated distillation tower according to claim 1 is characterized in that, described riser (12) is the 3-5 root.
6, a kind of chlorinated distillation tower according to claim 1 is characterized in that, the height of the logical chlorine tower joint of liquid phase (3) is 1.5-2.5 times of chlorination tower joint (4).
7, a kind of chlorinated distillation tower according to claim 1 is characterized in that, second Chlorination tube (10) is a 0.4-0.6 rice to the distance at downtake (11) top.
8, a kind of chlorinated distillation tower according to claim 1 is characterized in that, the pipeline that connects between chlorination tower (2), the distillation tower (1) is gas phase pipe and liquid phase upflow tube, all adopts enamel or inner liner polytetrafluoroethylene material conduit.
9, a kind of chlorinated distillation tower according to claim 1 is characterized in that, the afterbody of described first Chlorination tube (7) and second Chlorination tube (10) is equipped with gas distributor, and first Chlorination tube (7) is inserted into the bottom of chlorination tank (6).
CN 200520140008 2005-12-13 2005-12-13 Chlorinated distillating tower Expired - Fee Related CN2844120Y (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

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Granted publication date: 20061206

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