CN203513537U - P-benzoquinone cyclic crystallization device - Google Patents

P-benzoquinone cyclic crystallization device Download PDF

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Publication number
CN203513537U
CN203513537U CN201320525530.9U CN201320525530U CN203513537U CN 203513537 U CN203513537 U CN 203513537U CN 201320525530 U CN201320525530 U CN 201320525530U CN 203513537 U CN203513537 U CN 203513537U
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kettle
crystallization
pipe
tube
venturi tube
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CN201320525530.9U
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Chinese (zh)
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潘德华
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Xiantao City Health Science And Technology Ltd
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Xiantao City Health Science And Technology Ltd
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Abstract

The utility model discloses a p-benzoquinone cyclic crystallization device which comprises a crystallization kettle, a tower top condenser, a circulating pump and a PLC (programmable logic control) circuit, wherein one end of the tower top condenser is connected with a steam stripping tower top, and the other end of the tower top condenser is connected with a cylindrical section of a Venturi tube; the bottom of the Venturi tube is connected with a first material feeding tube of the crystallization kettle through a down-flow tube; a material discharging tube at the bottom of the crystallization kettle is connected with the circulating pump through a pipeline; a material discharging tube of the circulating pump is connected with a material feeding tube at the top of the Venturi tube through a pipeline and a Venturi tube material feeding valve. The p-benzoquinone cyclic crystallization device prevents non-condensable gas from being gathered at the tower top under the action of negative pressure suction of the Venturi tube, so that the temperature of the steam stripping tower top is reduced, self-aggregation coking of p-benzoquinone is avoided, and the purity of a product is improved. The down-flow tube is continuously flushed by crystalline mixed liquid, so that the phenomenon that the tube wall of the down-flow tube is blocked due to adhered crystallization can be avoided.

Description

Para benzoquinone circulation crystallization device
Technical field
The utility model relates to a kind of industrial chemicals gas stripping process, especially relates to a kind of para benzoquinone circulation crystallization device.
Background technology
Benzoquinones (benzoquinone) is a kind of of quinone.Molecular formula C6H4O2, has two kinds of adjacent benzoquinones and para benzoquinone.Para benzoquinone is more important, can be used as dyestuff and medicine intermediate, rubber antioxidant, stopper, antioxidant, photographic developer etc.
The conventional production methods of para benzoquinone is oxidation style, and aniline oxidation solution water at atmospheric pressure steam stripped is prepared para benzoquinone finished product.It is to adopt high-temperature vapor stripping that existing para benzoquinone extracts, and temperature is up to 100-110 ℃, but para benzoquinone is at high temperature unstable, can be further oxided into cis-butenedioic anhydride class impurity or autohemagglutination coking, reduces the yield of product.For preventing stripping coking, some enterprise has carried out some improvement to existing installation, as the patent No. a kind of decompression gas stripping process that is 200610125180, what adopt is that vacuum pump and crystallizer connect, water vapour containing para benzoquinone enters crystallizer by condenser, generate or reduction para benzoquinone, but after temperature reduction, the pipe wall that connects condenser and crystallizer easily adheres to crystallization and causes stopping up, equipment cannot normally be worked, and the solid-liquid separation after para benzoquinone condensation-crystallization cannot be carried out continuously.For improving the yield of para benzoquinone, above-mentioned deficiency need to be improved.
Summary of the invention
The utility model object is to provide a kind of para benzoquinone circulation crystallization device, with improve existing installation structure not too rationally, the technical problem such as the easy Crystallization Plugging of downtake, stripping production efficiency be low.
In order to solve the problems of the technologies described above, the technical solution adopted in the utility model is: a kind of para benzoquinone circulation crystallization device, comprises crystallization kettle, overhead condenser, recycle pump, PLC pilot circuit; Described overhead condenser one end is connected with stripping tower top, the overhead condenser the other end is connected with Venturi tube cylindrical section, Venturi tube bottom is connected with the first feed-pipe of crystallization kettle by downtake, the discharge nozzle of crystallization kettle bottom is connected with recycle pump by pipeline, recycle pump discharge nozzle by pipeline, Venturi tube feed valve, be connected with Venturi tube its top feed pipe.
As preferably, the discharge nozzle of described recycle pump is also connected with the feed-pipe of cyclone separator by pipeline; Cyclone separator top is provided with mother liquor delivery pipe, cyclone separator bottom is provided with crystallization mixture delivery pipe, mother liquor delivery pipe is connected with Venturi tube its top feed pipe, crystallization mixture delivery pipe is connected with horizontal centrifuge feed-pipe with whizzer feed valve by pipeline, and the whizzer drain pipe of whizzer bottom is connected with the second feed-pipe of crystallization kettle by pipeline.
As preferably, described crystallization kettle comprises kettle, and crystallization kettle kettle consists of internal layer still wall and outer still wall, between internal layer still wall and outer still wall, forms chuck layer, outer still wall is provided with water coolant inhalent siphon and cooling water outlet pipe, and water coolant inhalent siphon and cooling water outlet pipe are communicated with chuck layer; Kettle top is provided with the first feed-pipe, and autoclave body bottom is provided with crystallization kettle discharge nozzle; Kettle inside is provided with spiral helicine electric heating tube, kettle top is provided with speed reduction unit, speed reduction unit top is provided with electric motor, motor output shaft is connected with reducer input shaft, reducer output shaft is connected with the vertical rotation axis in kettle, on vertical rotation axis, be provided with many group oar formula agitating vanes, oar formula agitating vane edge is provided with a plurality of flow-disturbings hole; Electric heating tube is looped around around oar formula agitating vane; On internal layer still wall, be provided with pressure transmitter, autoclave body bottom and overhead condenser are provided with temperature sensor.
As preferably, described temperature sensor, pressure transmitter are connected with the input terminus of PLC pilot circuit, and the control end of PLC pilot circuit is connected with electric heating tube, electric motor, recycle pump.
The utility model is to increase Venturi tube on traditional gas stripping process, makes recycle pump, Venturi tube, crystallization kettle interconnection, by the negative pressure-pumping effect of Venturi tube, prevent tower top gathering non-condensable gases, reduce stripping tower head temperature, avoid the coking of para benzoquinone autohemagglutination, improve product purity.The continuous circulation scouring downtake of crystallization mixture, can avoid downtake tube wall to adhere to crystallization and cause stopping up.The water vapor that contains para benzoquinone and crystallization mixture hybrid cooling, can make crystallization color bright orange, improves the quality of crystallization.This technique can well be improved the deficiency of existing installation, improves para benzoquinone output, has good economic benefit.
Accompanying drawing explanation
Fig. 1 is structural representation of the present utility model;
Fig. 2 is the structural representation of crystallization kettle;
Fig. 3 is the schematic diagram of PLC pilot circuit.
Embodiment
Below in conjunction with the drawings and specific embodiments, the technical solution of the utility model is described in further detail.Fig. 1 is structural representation of the present utility model, and Fig. 2 is the structural representation of crystallization kettle, and Fig. 3 is the schematic diagram of PLC pilot circuit.
As seen from the figure, realize the equipment of para benzoquinone condensation-crystallization technique, comprise crystallization kettle 1, cyclone separator 3, horizontal centrifuge 4, overhead condenser 5, Venturi tube 6, PLC pilot circuit 7 etc.Overhead condenser 5 one end are connected with stripping tower top, and overhead condenser 5 the other ends are connected with Venturi tube 6 cylindrical sections, and Venturi tube 6 bottoms are connected with the first feed-pipe 13 of crystallization kettle 1 by downtake 61.Crystallization kettle 1 comprises kettle 101, crystallization kettle kettle 101 is surrounded and is formed by internal layer still wall 11 and outer still wall 12, between internal layer still wall 11 and outer still wall 12, form chuck layer 10, outer still wall 12 is provided with water coolant inhalent siphon 111 and cooling water outlet pipe 112, and water coolant inhalent siphon 111 and cooling water outlet pipe 112 are communicated with chuck layer 10.Kettle 101 inside are provided with spiral helicine electric heating tube 16, kettle 101 tops are provided with speed reduction unit 21, speed reduction unit top 21 is provided with electric motor 22, electric motor 22 output shafts are connected with speed reduction unit 21 input shafts, speed reduction unit 21 output shafts are connected with the vertical rotation axis 23 in kettle 101, on vertical rotation axis 23, be provided with many group oar formula agitating vanes 24, oar formula agitating vane 24 edges are provided with a plurality of flow-disturbings hole 25.Electric heating tube 16 is looped around around oar formula agitating vane 24.On internal layer still wall 11, be provided with pressure transmitter 17, kettle 101 bottoms and overhead condenser 4 are provided with temperature sensor 18.The discharge nozzle 15 of crystallization kettle 1 bottom is connected with recycle pump 26 by pipeline, recycle pump 26 discharge nozzle by pipeline, Venturi tube feed valve 27, be connected with Venturi tube 3 its top feed pipes.Temperature sensor 18, pressure transmitter 17 are connected with the input terminus of PLC pilot circuit 7, and the control end of PLC pilot circuit 7 is connected with electric heating tube 16, electric motor 22, recycle pump 26.
Embodiment: when opening Venturi tube feed valve 27, while closing cyclone separator control valve 271,272, the water vapor that contains gas phase para benzoquinone at stripping tower top is under the negative pressure-pumping effect of Venturi tube 6, by near the condenser 5 stripping tower top, to the interior logical hot water of condenser 5, make water vapor be cooled to 80-100 ℃.Water vapor by condenser 5 is sent in crystallization kettle 1 through Venturi tube 6 and downtake 61, in the chuck layer 10 of crystallization kettle 1, pass into frozen water, make the temperature in crystallization kettle 1 be down to 0-20 ℃, crystallization kettle 1 is by steps such as 24 stirrings of oar formula agitating vane, cooling water circulation quenchings, para benzoquinone is separated out, the crystallization mixture of crystallization kettle 1 interior generation with crystal habit.The lower concentration crystallization mixture that contains para benzoquinone crystallization is delivered to Venturi tube 6 through crystallization kettle discharge nozzle 15, recycle pump 26, that at Venturi tube 6 intercrystalline mixed solutions, sends into overhead condenser 5 mixes containing para benzoquinone water vapor, sends into crystallization kettle 1 again carry out crystallization through downtake 61.
Finally, it should be pointed out that above embodiment is only the more representational example of the utility model.Obviously, the utility model is not limited to above-mentioned embodiment, can also have many distortion.Any simple modification, equivalent variations and modification that every foundation technical spirit of the present utility model is done above embodiment, all should think and belong to protection domain of the present utility model.

Claims (4)

1. a para benzoquinone circulation crystallization device, comprises crystallization kettle, overhead condenser, recycle pump, PLC pilot circuit; It is characterized in that described overhead condenser one end is connected with stripping tower top, the overhead condenser the other end is connected with Venturi tube cylindrical section, Venturi tube bottom is connected with the first feed-pipe of crystallization kettle by downtake, the discharge nozzle of crystallization kettle bottom is connected with recycle pump by pipeline, recycle pump discharge nozzle by pipeline, Venturi tube feed valve, be connected with Venturi tube its top feed pipe.
2. para benzoquinone circulation crystallization device according to claim 1, is characterized in that the discharge nozzle of described recycle pump is also connected with the feed-pipe of cyclone separator by pipeline; Cyclone separator top is provided with mother liquor delivery pipe, cyclone separator bottom is provided with crystallization mixture delivery pipe, mother liquor delivery pipe is connected with Venturi tube its top feed pipe, crystallization mixture delivery pipe is connected with horizontal centrifuge feed-pipe with whizzer feed valve by pipeline, and the whizzer drain pipe of whizzer bottom is connected with the second feed-pipe of crystallization kettle by pipeline.
3. para benzoquinone circulation crystallization device according to claim 1, it is characterized in that described crystallization kettle comprises kettle, crystallization kettle kettle consists of internal layer still wall and outer still wall, between internal layer still wall and outer still wall, form chuck layer, outer still wall is provided with water coolant inhalent siphon and cooling water outlet pipe, and water coolant inhalent siphon and cooling water outlet pipe are communicated with chuck layer; Kettle top is provided with the first feed-pipe, and autoclave body bottom is provided with crystallization kettle discharge nozzle; Kettle inside is provided with spiral helicine electric heating tube, kettle top is provided with speed reduction unit, speed reduction unit top is provided with electric motor, motor output shaft is connected with reducer input shaft, reducer output shaft is connected with the vertical rotation axis in kettle, on vertical rotation axis, be provided with many group oar formula agitating vanes, oar formula agitating vane edge is provided with a plurality of flow-disturbings hole; Electric heating tube is looped around around oar formula agitating vane; On internal layer still wall, be provided with pressure transmitter, autoclave body bottom and overhead condenser are provided with temperature sensor.
4. para benzoquinone circulation crystallization device according to claim 3, is characterized in that described temperature sensor, pressure transmitter are connected with the input terminus of PLC pilot circuit, and the control end of PLC pilot circuit is connected with electric heating tube, electric motor, recycle pump.
CN201320525530.9U 2013-08-27 2013-08-27 P-benzoquinone cyclic crystallization device Expired - Lifetime CN203513537U (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103497099A (en) * 2013-08-27 2014-01-08 仙桃市康化科技有限公司 p-benzoquinone condensation crystallization technology
CN105688729A (en) * 2016-04-13 2016-06-22 赵扬 Hydromechanical auto-control three-stage mixing equipment
CN106748702A (en) * 2017-01-17 2017-05-31 湖北开元化工科技股份有限公司 The equipment that a kind of sublimed method produces 1,4-benzoquinone

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103497099A (en) * 2013-08-27 2014-01-08 仙桃市康化科技有限公司 p-benzoquinone condensation crystallization technology
CN103497099B (en) * 2013-08-27 2015-07-01 仙桃市康化科技有限公司 p-benzoquinone condensation crystallization technology
CN105688729A (en) * 2016-04-13 2016-06-22 赵扬 Hydromechanical auto-control three-stage mixing equipment
CN105688729B (en) * 2016-04-13 2019-03-01 赵扬 The three-level mixing device of hydrodynamics automatic control
CN106748702A (en) * 2017-01-17 2017-05-31 湖北开元化工科技股份有限公司 The equipment that a kind of sublimed method produces 1,4-benzoquinone
CN106748702B (en) * 2017-01-17 2023-09-01 湖北开元化工科技股份有限公司 Equipment for producing p-benzoquinone by sublimation method

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Granted publication date: 20140402