CN103480176A - Continuous separation device for p-benzoquinone crystals - Google Patents
Continuous separation device for p-benzoquinone crystals Download PDFInfo
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- CN103480176A CN103480176A CN201310377851.3A CN201310377851A CN103480176A CN 103480176 A CN103480176 A CN 103480176A CN 201310377851 A CN201310377851 A CN 201310377851A CN 103480176 A CN103480176 A CN 103480176A
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Abstract
The invention relates to a continuous separation device for p-benzoquinone crystals. The continuous separation device comprises a crystallizing kettle, a cyclone separator, a horizontal centrifuge and a PLC (Programmable Logic Controller) control circuit. The continuous separation device has the advantages of energy conservation, environment friendliness and high production efficiency; a mixed liquid containing the p-benzoquinone crystals is subjected to warming, stirring and shock cooling by virtue of the crystallizing kettle so as to generate products, the products are conveyed to the cyclone separator through a discharging pipe of the crystallizing kettle, the mixed liquid containing the high-concentration crystals is conveyed to the horizontal centrifuge from the bottom of the cyclone separator and is subjected to solid-liquid separation, a p-benzoquinone mother solution is conveyed to a water film generator at the upper part of a p-benzoquinone stripping tower from the top of the cyclone separator or returns into the crystallizing kettle, and a mother solution separated by the horizontal centrifuge returns into the crystallizing kettle as well; the processes are continuously and circularly carried out, so that the continuous separation of the p-benzoquinone crystals and the cycle use of the mother solution can be finished, and the outward draining is avoided. According to the continuous separation device, the problems that an existing device cannot continuously work and is low in efficiency are well solved, and the continuous separation device has excellent economic and social benefits.
Description
Technical field
The present invention relates to a kind of chemical industry equipment, especially relate to the continuous separation equipment of a kind of 1,4-benzoquinone crystallization.
Background technology
Benzoquinones (benzoquinone) is a kind of of quinone.Molecular formula C6H4O2, have two kinds of adjacent benzoquinones and 1,4-benzoquinone.1,4-benzoquinone is more important, can be used as dyestuff and medicine intermediate, rubber antioxidant, polymerization inhibitor, antioxidant, developer etc.
The conventional production methods of 1,4-benzoquinone is oxidizing process, and aniline oxidation solution water at atmospheric pressure steam stripping prepares the 1,4-benzoquinone finished product.Existing 1,4-benzoquinone extraction equipment design is reasonable not, needs a large amount of crystallization waters that use during its work, and the mother liquor of discharge is more, and pollutant emission is also more; Crystallization kettle is discontinuous operation often, carries out the Crystallization Separation operation after handling a still material again, and stripper is intermittently to use, and utilization rate of equipment and installations is lower, has caused like this decline of production efficiency.
Summary of the invention
The object of the invention is to provide the continuous separation equipment of a kind of 1,4-benzoquinone crystallization, with improve the existing equipment structure not too rationally, the technical problem such as more, the stripper of pollutant emission can not continuous operation, production efficiency is low.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is: the continuous separation equipment of a kind of 1,4-benzoquinone crystallization, comprise crystallization kettle, cyclone separator, horizontal centrifuge, PLC control circuit, described crystallization kettle comprises kettle, kettle top is provided with the first feed pipe, the second feed pipe, and autoclave body bottom is provided with the crystallization kettle discharge nozzle; The crystallization kettle discharge nozzle is connected with the feed pipe of circulating pump by pipeline, and the discharge nozzle of circulating pump is connected with the feed pipe of cyclone separator by pipeline; The cyclone separator top is provided with the mother liquor delivery pipe, the cyclone separator bottom is provided with the crystallization mixture delivery pipe, the mother liquor delivery pipe is connected with three-way pipe one end, and the other two ends of three-way pipe are connected with crystallization kettle the first feed pipe with 1,4-benzoquinone stripper top moisture film generating means respectively by pipeline; The crystallization mixture delivery pipe is connected with the horizontal centrifuge feed pipe with the centrifuge inlet valve by pipeline, and the centrifuge drain pipe of centrifuge bottom is connected with the second feed pipe of crystallization kettle by pipeline.
As preferably, described crystallization kettle kettle consists of internal layer still wall and outer still wall, form the chuck layer between internal layer still wall and outer still wall, outer still wall is provided with cooling water oral siphon and cooling water outlet pipe, cooling water oral siphon and cooling water outlet pipe are communicated with the chuck layer, kettle inside is provided with spiral helicine electric heating tube, the kettle top is provided with decelerator, the decelerator top is provided with motor, described motor output shaft is connected with reducer input shaft, reducer output shaft is connected with the vertical rotation axis in kettle, be provided with many group oar formula stirring vanes on vertical rotation axis, oar formula stirring vane edge is provided with a plurality of flow-disturbings hole, electric heating tube is looped around around oar formula stirring vane, also be provided with pressure sensor on described internal layer still wall, autoclave body bottom is provided with temperature sensor.
As preferably, described horizontal centrifuge comprises casing, rotary drum, support, differential mechanism, and described bottom of shell is provided with centrifuge drain pipe and 1,4-benzoquinone crude product delivery pipe, be provided with rotary drum in described casing, surface, rotary drum left side is provided with spout hole, right-hand part is provided with mud hole, the rotary drum two ends are provided with back shaft, described back shaft is respectively through the casing two ends, its end is fixed in the bearing block at support top, be provided with auger conveyor in described rotary drum, auger conveyor comprises main shaft and the winding helical blade on main shaft, be provided with the storing cavity in described main shaft, a described main shaft left side, right both sides are provided with rotating shaft, this left side, right spindle is located in respectively a rotary drum left side, in the back shaft at right two ends, wherein in the rotating shaft of right side, be penetrated with feed pipe, this feed pipe outer end is connected with the crystallization mixture delivery pipe of cyclone separator by pipeline, the end of feed pipe is positioned at the storing cavity, the storing cavity is communicated with rotary drum by the discharging opening on main shaft, described rotary drum left side back shaft, auger conveyor left side rotating shaft is connected with two groups of differential rotating shafts of differential mechanism respectively.
As preferably, described rotary drum left side is cylindrical segment, and rotary drum cylindrical segment surface is provided with spout hole, and the rotary drum right-hand part is conical section, and its conical section end is provided with the mud hole corresponding with residue outlet.
As preferably, described 1,4-benzoquinone stripper top moisture film generating means, comprise stripper, the seam of stripper top has the endless tube of a ring around stripper, endless tube is provided with the mother liquor entrance, be provided with some mother liquor outlets on stripper tower wall in the zone covered at endless tube, this mother liquor outlet is communicated with fully with endless tube, in endless tube, near the mother liquor exit, is provided with buffer board.
As preferably, described temperature sensor, pressure sensor are connected with the input of PLC control circuit, and the control end of PLC control circuit is connected with electric heating tube, motor, circulating pump, differential mechanism, centrifuge inlet valve.
The present invention has energy-conserving and environment-protective, the advantage that production efficiency is high, the intensification of the mixed liquor process crystallization kettle that contains the 1,4-benzoquinone crystallization-stirring-quenching, product is delivered to cyclone separator by the crystallization kettle discharge nozzle, deliver to horizontal centrifuge containing the mixed liquor of high concentration crystallization by the cyclone separator bottom and carry out Separation of Solid and Liquid, the 1,4-benzoquinone mother liquor is delivered to 1,4-benzoquinone stripper top moisture film generating means or is returned in crystallization kettle by the cyclone separator top, the mother liquor that the horizontal centrifuge sub-argument goes out also returns to crystallization kettle, said process constantly circulates, the continuous separate that can complete the 1,4-benzoquinone crystallization from the recycling of mother liquor, stopped external draining.This invention has well improved existing equipment can not continuous operation and the problem of inefficiency, has good economic benefit and a social benefit.
The accompanying drawing explanation
Fig. 1 is structural representation of the present invention;
Fig. 2 is the structural representation of crystallization kettle;
Fig. 3 is the structural representation of cyclone separator;
Fig. 4 is the structural representation of horizontal centrifuge;
Fig. 5 is the structural representation of Rotator of Horizontal Centrifuger;
Fig. 6 is the structural representation of 1,4-benzoquinone stripper top moisture film generating means;
Fig. 7 is the schematic diagram of PLC control circuit.
The specific embodiment
Below in conjunction with the drawings and specific embodiments, technical scheme of the present invention is described in further detail.Fig. 1 is structural representation of the present invention, Fig. 2 is the structural representation of crystallization kettle, Fig. 3 is the structural representation of cyclone separator, Fig. 4 is the structural representation of horizontal centrifuge, Fig. 5 is the structural representation of Rotator of Horizontal Centrifuger, Fig. 6 is the structural representation of 1,4-benzoquinone stripper top moisture film generating means, and Fig. 7 is the schematic diagram of PLC control circuit.
As seen from the figure, the continuous separation equipment of this 1,4-benzoquinone crystallization, comprise crystallization kettle 1, cyclone separator 3, horizontal centrifuge 4, PLC control circuit etc.Crystallization kettle 1 comprises kettle 101, crystallization kettle kettle 101 consists of internal layer still wall 11 and outer still wall 12, form chuck layer 10 between internal layer still wall 11 and outer still wall 12, outer still wall 12 is provided with cooling water oral siphon 111 and cooling water outlet pipe 112, and cooling water oral siphon 111 and cooling water outlet pipe 112 are communicated with chuck layer 10.Kettle 101 tops are provided with the first feed pipe 13, the second feed pipe 14, and kettle 101 bottoms are provided with crystallization kettle discharge nozzle 15.Kettle 101 inside are provided with spiral helicine electric heating tube 16, kettle 101 tops are provided with decelerator 21, decelerator top 21 is provided with motor 22, motor 22 output shafts are connected with decelerator 21 power shafts, decelerator 21 output shafts are connected with the vertical rotation axis 23 in kettle 101, be provided with many group oar formula stirring vanes 24 on vertical rotation axis 23, oar formula stirring vane 24 edges are provided with a plurality of flow-disturbings hole 25.Electric heating tube 16 is looped around around oar formula stirring vane 24; Also be provided with pressure sensor 17 on internal layer still wall 11, kettle 101 bottoms are provided with temperature sensor 18.
Crystallization kettle discharge nozzle 15 is connected with the feed pipe of circulating pump 26 by pipeline, and the discharge nozzle of circulating pump 26 is connected with the feed pipe 30 of cyclone separator 3 by pipeline; Cyclone separator 3 tops are provided with mother liquor delivery pipe 31, cyclone separator 3 bottoms are provided with crystallization mixture delivery pipe 32, mother liquor delivery pipe 31 is connected with three-way pipe 33, and the other two ends of three-way pipe 33 are connected with crystallization kettle the first feed pipe 13 with 1,4-benzoquinone stripper top moisture film generating means 5 respectively; Crystallization mixture delivery pipe 32 is connected with horizontal centrifuge feed pipe 44 with centrifuge inlet valve 34 by pipeline.
1,4-benzoquinone stripper top moisture film generating means 5 is included in the endless tube 53 of a ring of stripper 52 top seam around stripper 52, endless tube 53 is provided with some mother liquor entrances 54, be provided with some mother liquor outlets 51 on stripper 52 tower walls in the zone covered at endless tube 53, mother liquor outlet 51 is uniformly distributed this mother liquor outlet 51 and is communicated with fully with endless tube 53 on stripper 52 walls, and the interior close mother liquor of endless tube 53 exports 51 places and is provided with buffer board 55.
Temperature sensor 18, pressure sensor 17 are connected with the input of PLC control circuit, and the control end of PLC control circuit is connected with electric heating tube 16, motor 22, circulating pump 26, differential mechanism 43, centrifuge inlet valve 34.
The effect of crystallization kettle 1 is by steps such as 24 stirrings of oar formula stirring vane, cooling water circulation quenchings, and 1,4-benzoquinone is separated out with crystal habit.The crystallization mixture that contains the 1,4-benzoquinone crystallization is delivered in cyclone separator 3 through crystallization kettle discharge nozzle 15, circulating pump 26, and the mother liquor that proportion is little is delivered to 1,4-benzoquinone stripper top moisture film generating means 5 or returned in crystallization kettle 1 by the first feed pipe 13 by the mother liquor delivery pipe 31 at top.The dense crystallization mixture of heavy height is delivered in horizontal centrifuge 4 by crystallization mixture delivery pipe 32, centrifuge inlet valve 34, rotary drum 1 and auger conveyor 45 are relative motion under the effect of differential mechanism 43, and the 1,4-benzoquinone mother liquor can be discharged and be sent back in crystallization kettle 1 by centrifuge drain pipe 461, the second feed pipe 14 from rotary drum 41.Crystallization meeting in material is delivered to rotary drum 41 tapering points at auger conveyor 45, and 1,4-benzoquinone crude product delivery pipe 462 scrapes, and enters the subsequent treatment operation, to obtain highly purified 1,4-benzoquinone.This equipment can make stripper 52 continuous operations, improves steam stripping efficiency.Horizontal centrifuge 4 chargings adopt sequence valve to control, and stop charging when crystallization scrapes, and recover charging after crystallization scrapes.Mother liquor can be used by iterative cycles in equipment, farthest reduces the crystallization water, has saved production cost, has reduced emission, is conducive to environmental protection.
Finally, it should be pointed out that the above specific embodiment is only the more representational example of the present invention.Obviously, the invention is not restricted to the above-mentioned specific embodiment, many distortion can also be arranged.Any simple modification, equivalent variations and modification that every foundation technical spirit of the present invention is done the above specific embodiment, all should think and belong to protection scope of the present invention.
Claims (6)
1. the continuous separation equipment of 1,4-benzoquinone crystallization, comprise crystallization kettle, cyclone separator, horizontal centrifuge, PLC control circuit, it is characterized in that described crystallization kettle comprises kettle, kettle top is provided with the first feed pipe, the second feed pipe, and autoclave body bottom is provided with the crystallization kettle discharge nozzle; The crystallization kettle discharge nozzle is connected with the feed pipe of circulating pump by pipeline, and the discharge nozzle of circulating pump is connected with the feed pipe of cyclone separator by pipeline; The cyclone separator top is provided with the mother liquor delivery pipe, the cyclone separator bottom is provided with the crystallization mixture delivery pipe, the mother liquor delivery pipe is connected with three-way pipe one end, and the other two ends of three-way pipe are connected with crystallization kettle the first feed pipe with 1,4-benzoquinone stripper top moisture film generating means respectively by pipeline; The crystallization mixture delivery pipe is connected with the horizontal centrifuge feed pipe with the centrifuge inlet valve by pipeline, and the centrifuge drain pipe of centrifuge bottom is connected with the second feed pipe of crystallization kettle by pipeline.
2. the continuous separation equipment of a kind of 1,4-benzoquinone crystallization according to claim 1, it is characterized in that described crystallization kettle kettle consists of internal layer still wall and outer still wall, form the chuck layer between internal layer still wall and outer still wall, outer still wall is provided with cooling water oral siphon and cooling water outlet pipe, cooling water oral siphon and cooling water outlet pipe are communicated with the chuck layer, kettle inside is provided with spiral helicine electric heating tube, the kettle top is provided with decelerator, the decelerator top is provided with motor, described motor output shaft is connected with reducer input shaft, reducer output shaft is connected with the vertical rotation axis in kettle, be provided with many group oar formula stirring vanes on vertical rotation axis, oar formula stirring vane edge is provided with a plurality of flow-disturbings hole, electric heating tube is looped around around oar formula stirring vane, also be provided with pressure sensor on described internal layer still wall, autoclave body bottom is provided with temperature sensor.
3. the continuous separation equipment of a kind of 1,4-benzoquinone crystallization according to claim 1, is characterized in that described horizontal centrifuge comprises casing, rotary drum, support, differential mechanism, and described bottom of shell is provided with centrifuge drain pipe and 1,4-benzoquinone crude product delivery pipe, be provided with rotary drum in described casing, surface, rotary drum left side is provided with spout hole, right-hand part is provided with mud hole, the rotary drum two ends are provided with back shaft, described back shaft is respectively through the casing two ends, its end is fixed in the bearing block at support top, be provided with auger conveyor in described rotary drum, auger conveyor comprises main shaft and the winding helical blade on main shaft, be provided with the storing cavity in described main shaft, a described main shaft left side, right both sides are provided with rotating shaft, this left side, right spindle is located in respectively a rotary drum left side, in the back shaft at right two ends, wherein in the rotating shaft of right side, be penetrated with feed pipe, this feed pipe outer end is connected with the crystallization mixture delivery pipe of cyclone separator by pipeline, the end of feed pipe is positioned at the storing cavity, the storing cavity is communicated with rotary drum by the discharging opening on main shaft, described rotary drum left side back shaft, auger conveyor left side rotating shaft is connected with two groups of differential rotating shafts of differential mechanism respectively.
4. the continuous separation equipment of a kind of 1,4-benzoquinone crystallization according to claim 3, it is characterized in that described rotary drum left side is cylindrical segment, rotary drum cylindrical segment surface is provided with spout hole, and the rotary drum right-hand part is conical section, and its conical section end is provided with the mud hole corresponding with residue outlet.
5. the continuous separation equipment of a kind of 1,4-benzoquinone crystallization according to claim 1, it is characterized in that described 1,4-benzoquinone stripper top moisture film generating means, comprise stripper, the seam of stripper top has the endless tube of a ring around stripper, endless tube is provided with the mother liquor entrance, be provided with some mother liquor outlets on stripper tower wall in the zone covered at endless tube, this mother liquor outlet is communicated with fully with endless tube, in endless tube, near the mother liquor exit, is provided with buffer board.
6. according to the continuous separation equipment of the described a kind of 1,4-benzoquinone crystallization of claim 2 or 3, it is characterized in that described temperature sensor, pressure sensor are connected with the input of PLC control circuit, the control end of PLC control circuit is connected with electric heating tube, motor, circulating pump, differential mechanism, centrifuge inlet valve.
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Cited By (7)
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CN105381776A (en) * | 2015-12-17 | 2016-03-09 | 常熟市水处理助剂厂有限公司 | Temperature controllable corrosion inhibition scale inhibitor preparation reactor |
CN105709864A (en) * | 2016-04-28 | 2016-06-29 | 黄尚勋 | Self-bed ion exchanger capable of automatically removing scars by using anti-locking effect of centrifugal force field |
CN104761440B (en) * | 2014-09-17 | 2017-06-23 | 中国科学院青岛生物能源与过程研究所 | A kind of separation/purification method of 1,4-benzoquinone compound |
CN107308678A (en) * | 2017-06-19 | 2017-11-03 | 青海盐湖工业股份有限公司 | A kind of automatic control system of crystallizer |
CN108203080A (en) * | 2018-03-07 | 2018-06-26 | 张炳文 | A kind of quenching device and its application method |
CN111939590A (en) * | 2020-08-22 | 2020-11-17 | 江西永宁科技有限责任公司 | High-vacuum low-temperature crystallization equipment for producing potassium perchlorate and use method thereof |
CN113717114A (en) * | 2021-09-23 | 2021-11-30 | 济南悟通生物科技有限公司 | 2-acetylpyrazine continuous recrystallization device, method and application thereof |
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2013
- 2013-08-27 CN CN201310377851.3A patent/CN103480176A/en active Pending
Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104761440B (en) * | 2014-09-17 | 2017-06-23 | 中国科学院青岛生物能源与过程研究所 | A kind of separation/purification method of 1,4-benzoquinone compound |
CN105381776A (en) * | 2015-12-17 | 2016-03-09 | 常熟市水处理助剂厂有限公司 | Temperature controllable corrosion inhibition scale inhibitor preparation reactor |
CN105709864A (en) * | 2016-04-28 | 2016-06-29 | 黄尚勋 | Self-bed ion exchanger capable of automatically removing scars by using anti-locking effect of centrifugal force field |
CN107308678A (en) * | 2017-06-19 | 2017-11-03 | 青海盐湖工业股份有限公司 | A kind of automatic control system of crystallizer |
CN108203080A (en) * | 2018-03-07 | 2018-06-26 | 张炳文 | A kind of quenching device and its application method |
CN111939590A (en) * | 2020-08-22 | 2020-11-17 | 江西永宁科技有限责任公司 | High-vacuum low-temperature crystallization equipment for producing potassium perchlorate and use method thereof |
CN113717114A (en) * | 2021-09-23 | 2021-11-30 | 济南悟通生物科技有限公司 | 2-acetylpyrazine continuous recrystallization device, method and application thereof |
CN113717114B (en) * | 2021-09-23 | 2022-12-02 | 济南悟通生物科技有限公司 | 2-acetylpyrazine continuous recrystallization device, method and application thereof |
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