CN102430261B - Continuous cooling crystallizer - Google Patents
Continuous cooling crystallizer Download PDFInfo
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- CN102430261B CN102430261B CN201110269347.2A CN201110269347A CN102430261B CN 102430261 B CN102430261 B CN 102430261B CN 201110269347 A CN201110269347 A CN 201110269347A CN 102430261 B CN102430261 B CN 102430261B
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- heat exchanger
- hollow shaft
- crystallization tank
- cooling medium
- exchanger tube
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Abstract
The invention discloses a continuous cooling crystallizer, comprising a crystallization tank and a heat exchanger in the crystallization tank, wherein, the heat exchanger comprises a top-enclosed heat exchange cylinder, a heat exchange pipe fixed in the heat exchange cylinder, a cooling medium inlet pipe and a cooling medium outlet pipe; a hollow shaft vertically passing through the top surface of the crystallization tank and a driving mechanism driving the hollow shaft to rotate are arranged above the crystallization tank, the top end of the hollow shaft is connected with a three-channel rotary joint, the bottom end of the hollow shaft is connected with the enclosed end of the heat exchange cylinder; a material pipe which has a top end communicated with one channel of the three-channel rotary joint and a bottom end passing through the heat exchange cylinder is arranged in the hollow shaft, one ends of the cooling medium inlet pipe and the cooling medium outlet pipe are respectively communicated with the inlet end and outlet end of the heat exchange pipe, and the other ends of the cooling medium inlet pipe and the cooling medium outlet pipe are respectively communicated with the rest two channels of the three-channel rotary joint. The continuous cooling crystallizer is used in a cooled shell-and-tube heat exchanger and arranged in the crystallization tank, rotates at a certain speed when working, and the cooling process and stirring process are combined as a whole, thus the crystallization efficiency is greatly increased.
Description
Technical field
The present invention relates to a kind of chemical industry equipment, relate in particular to a kind of continuous cooling crystallizer.
Background technology
Crystallisation by cooling is by cooling solution, and the solubility that reduces solute becomes supersaturated solution, and separates out the process of solute, is applicable to that solubility with temperature declines and the material that significantly reduces.It can obtain very pure crystal product from the very high solution of impurity content, is applicable to many separated mixing system, isomerism system and thermal sensitivity systems of being difficult to.The material that chemical composition is identical, under different physical and chemical conditions, can crystallize into the crystal of two kinds or above different structure, and these crystal has different physics, chemical property, thus crystallization parameters be controlled in Chemical Manufacture very crucial.
Existing solution crystallization equipment is mainly kettle type crystallization device, comprises internal-circulation type cooler crystallizer and outer circulation type cooler crystallizer.What internal-circulation type cooler crystallizer was selected conventionally is the jacket type crystallization kettle that band stirs, and the required cold of crystallisation by cooling is provided by chuck, and heat exchange area is less, and heat exchange amount is little.Outer circulation type cooler crystallizer crystallization cold is provided by external heat exchanger conventionally.Heat transfer coefficient is large, and heat exchange area is variable, but must select suitable circulating pump, and the wearing and tearing of the crystal of avoiding suspending are broken, the easier fouling of external heat exchanger, thus impact is used.
Krystal-Oslo classifying crystallizer is common cooler crystallizer, and its supersaturation generation equipment is a cooling heat exchanger, and during crystallization, solution is by tube side (one-pass type is the most general), and cooling medium passes through shell side.When fresh cooling medium pours heat exchanger shell pass, very large with the solution temperature difference, and degree of supersaturation Jie Wen district is very narrow Yi Ge region, solution is easily in the fouling of cooling medium porch, must set up a set of auxiliary refrigerant cycle system, the degree of supersaturation that produces heat exchanger transfinites not only can occur in the two ends that tube side is imported and exported, and is subject to the impact of the inside and outside both sides of tube wall fluid situation.Need cryogen indirectly by auxiliary circulation system, to be cushioned for this reason.
Summary of the invention
The invention provides a kind of continuous cooling crystallizer, this mold structure is simple, and crystalline rate is high, stable performance.
, comprising the heat exchanger in crystallization tank and crystallization tank, described heat exchanger comprises that the heat exchanger tube of top closure, the heat exchanger tube that is fixed on heat exchanger tube inside, cooling medium inlet pipe and cooling medium go out pipe; Described crystallization tank top is provided with the driving mechanism vertically rotating through hollow shaft and the driving hollow shaft of crystallization tank end face, and hollow shaft top connects a three-way swivel joint, and bottom connects the blind end of heat exchanger tube; Hollow shaft inside be provided with that top is communicated with one of them path of three-way swivel joint and bottom through the materail tube of heat exchanger tube, cooling medium inlet pipe and cooling medium Chu Guan one end are communicated with entrance point and the port of export of heat exchanger tube respectively, the other end stretches in its cavity through hollow shaft sidewall, and is communicated with all the other two paths of three-way swivel joint respectively.
Described driving mechanism by motor, the driving-chain that is fixed on driving wheel on motor output shaft, is enclosed within the driven pulley in hollow shaft and connects driving wheel and driven pulley forms.
Described crystallization tank top is provided with the bearing support of fixation hollow axle, between described bearing support and hollow shaft, is provided with clutch shaft bearing.
Between described hollow shaft and crystallization tank, be provided with the second bearing and sealing ring, improve sealing property and bearing strength.
Described crystallization tank sidewall is provided with observation panel, is convenient to observe height of materials.
Described crystallization tank bottom is taper, and bottom connects a vertical material guiding tube, is convenient to material after crystallization to introduce separator.
Described heat exchanger tube vertically arranges.
1, crystallizer of the present invention is placed in crystallization tank inside for cooling shell-and-tube heat exchanger, and with certain speed, rotates during work, and cooling procedure and whipping process are blended in one, have greatly improved crystalline rate; And material with certain flow velocity from top to bottom by tube side, crystallizer inside is less scaling.
2, present device is simple in structure, stable operation, and for continuous production, efficiency is higher, also can be according to process conditions Batch Process.
3, crystallizer of the present invention can be used for Real-Time Monitoring, measures various technological parameters, investigates the mechanism of course of reaction, and midget plant can be used for carrying out scientific research.
Accompanying drawing explanation
Fig. 1 is the structural representation of continuous cooling crystallizer of the present invention.
Fig. 2 is crystallizer shown in Fig. 1 and ancillary equipment connection diagram.
The specific embodiment
As shown in Figure 1, a kind of continuous cooling crystallizer, comprises the heat exchanger in crystallization tank 1 and crystallization tank 1, and crystallization tank 1 is the flat-top cone container at the end, a plurality of observation panels 7 that are provided with on sidewall.Crystallization tank 1 cylindrical portions diameter is 1000mm, and length is 2500mm, tapering part height 500mm, and bottom connects material guiding tube 6.Heat exchanger comprises the heat exchanger tube 3 in heat exchanger tube 2 and heat exchanger tube 2, the snakelike tubulation that heat exchanger tube vertically arranges, and length is 150mm, is evenly covered with the inner chamber of whole heat exchanger tube 2, heat exchange area is about 10m
2, entrance point and the port of export, through heat exchanger tube 2 sidewalls, are fixed on heat exchanger tube 2 inside.Heat exchanger tube 2 diameter 400mm, there is a capping connecting by flange 17 on top, makes its top closure.
Crystallization tank 1 top is provided with the bearing support 8 of vertical hollow shaft 10 and fixation hollow axle 10, hollow shaft 10 external diameter 100mm, and internal diameter 60mm, is provided with bearing 16 between it and bearing support 8.Hollow shaft 10 connecting tee road, top swivel joints, bottom is fixedly connected with capping 17 through crystallization tank 1, in order to improve sealing property, between hollow shaft 10 and crystallization tank 1, has sealing ring 15.For improving bearing strength, between hollow shaft 10 and crystallization tank 1, be also provided with bearing 9.In the inner chamber of hollow shaft 10, be also provided with bottom through the materail tube 18 of capping 17, materail tube 18 calibers are 32mm.
Crystallization tank 1 end face is also set with support 12, is fixed with motor 13 on support 12, fixing driving wheel on motor 13 output shafts, and in hollow shaft 10, cover has driven pulley, between driving wheel and driven pulley, by driving-chain 11, connects.
Heat exchanger tube 2 both sides are provided with cooling medium inlet pipe 5, the cooling medium that caliber is 25mm and go out pipe 4, cooling medium inlet pipe 5 goes out pipe 4 one end with cooling medium and is connected with the port of export with the entrance point of heat exchanger tube 3 respectively, the other end penetrates the inner chamber of hollow shaft 10 and two paths of three-way swivel joint 14 are communicated with, and the path of three-way swivel joint 14 remainders is communicated with materail tube 18.
As shown in Figure 2, before work, three entrances of three-way swivel joint send device 20, cooling medium recover 21 by pipeline attachment material source 19, cooling medium respectively, and material guiding tube 6 connects centrifuge 22 by pipeline, is equipped with flowmeter and control valve on pipeline.
During work, the material that needs crystallization enters in crystallization tank 1 through the first path, the materail tube 18 of three-way swivel joint 14, observes the liquid level of the inside by observation panel 7, when liquid level reaches roughly crystallization tank height 2/3, open motor 13, heat exchanger is rotated.In rotation process, cooling medium from cooling medium send device 20 out, second path through three-way swivel joint 14, enter successively cooling medium inlet pipe 5, heat exchanger tube 3, cooling medium and go out pipe 4, finally the 3rd from three-way swivel joint 14 passes into away, gets back to cooling medium recover 21.
Cooling medium is when by heat exchanger tube 3, and the material generation heat exchange with in heat exchanger tube 2, makes material generation crystallization.After crystallization, the bottom that material enters crystallization tank 1 enters centrifuge 22 by drainage tube 6, and separation obtains crystalline solid.
Application examples 1
By temperature, be that 50 ℃ of Coumarin-6 3-(2-[4-morpholinodithio base)-7-lignocaine cumarin acetone soln enters from the import of swivel joint 14 with 1.5t/h, the tube side that enters heat exchanger through the materail tube 18 in the axis hole of hollow shaft 10, enters crystallization tank 1 by heat exchanger tube 2.By observing visor 7, when a half of crystallization tank 1 liquid level arrival crystallization tank 1 cylindrical shell height, open crystallization tank 1 bottom valve, solution enters centrifuge 22, regulates material imported valve simultaneously, guarantees level stability.
Starter motor 13 after stable, by driving-chain 11, drive hollow shaft 10 and whole heat exchanger to rotate with 100rpm speed, open cooling medium valve, chilled water enters by the cooling medium inlet of threeway swivel joint 14, after path of threeway swivel joint, enters cooling medium inlet pipe 5, then from heat exchanger bottom, enters shell side, and from heat exchanger top, get back to cooling medium and go out pipe 4, the passage by threeway swivel joint 14 enters cooling medium recover 21.
Observe the temperature of crystallization tank 1 outlet, regulate cooling medium consumption, outlet temperature reaches 15 ℃, reaches stable, and solution is through heat exchanger, temperature reduces rapidly, at heat exchanger exit, place becomes supersaturated solution, and Coumarin-6 3-(2-[4-morpholinodithio base)-7-lignocaine cumarin crystal is separated out from solution, because Action of Gravity Field layer drops to crystallization tank 1 bottom, crystal and solution enter centrifuge 22 separation by bottom valve, obtain the pure crystal of epigranular.
State Behavior of Continuous Crystallization Processes is compared with the K3000L enamel autoclave crystallizer that conventional band stirs, and crystalline rate obviously improves.Adopt kettle type crystallization device, process 3m
3solution needs 4～5h, adopts the present invention only to need 2h just to complete crystallization, and crystal amount is than adopting conventional crystallizer how about 10%.
Application examples 2
The Sodium.beta.-phenylpyruvate methanol solution that is 45 ℃ by temperature enters from the material inlet of threeway swivel joint 14 with 1.5t/h, through materail tube 18, enter the tube side of heat exchanger, by heat exchanger tube, enter crystallization tank 1, by observing visor 7, when crystallization tank 1 liquid level arrives three of a crystallization tank 1 shell portion height/for the moment, open the valve of crystallization tank 1 bottom, solution enters centrifuge 22.
Starter motor 13 after level stability, by driving-chain 11, drive hollow shaft 10 and whole heat exchanger to rotate with 85rpm speed, open cooling medium valve, chilled brine enters by the cooling medium inlet 13 of threeway swivel joint 14, enters cooling medium inlet pipe 4 after one of them path, then from heat exchanger bottom, enters shell side, and from heat exchanger top, return cooling medium and go out pipe 4, another passage by swivel joint 14 enters cooling medium recover 21.
Observe the temperature of crystallization tank 1 outlet, regulate cooling medium consumption, outlet temperature reaches 8 ℃, reach stable, solution is through heat exchanger, and temperature reduces rapidly, phenylpyruvic acid sodium crystal is separated out from solution, because Action of Gravity Field layer drops to crystallization tank bottom, crystal and solution enter centrifuge 22 separation by bottom valve, obtain the pure crystal of epigranular.
State Behavior of Continuous Crystallization Processes of the present invention is compared with the K5000L enamel autoclave crystallizer (jacketed) that conventional band stirs, and crystalline rate obviously improves.Adopt kettle type crystallization device, process 5m
3solution needs 5～6h, adopts this patent approximately to need 3.5h just to complete crystallization, and crystal amount is than adopting conventional crystallizer how about 8%.
Claims (8)
1. a continuous cooling crystallizer, comprises the heat exchanger in crystallization tank and crystallization tank, it is characterized in that, described heat exchanger comprises that the heat exchanger tube of top closure, the heat exchanger tube that is fixed on heat exchanger tube inside, cooling medium inlet pipe and cooling medium go out pipe; Described crystallization tank top is provided with the driving mechanism vertically rotating through hollow shaft and the driving hollow shaft of crystallization tank end face, and hollow shaft top connects a three-way swivel joint, and bottom connects the blind end of heat exchanger tube; Hollow shaft inside be provided with that top is communicated with one of them path of three-way swivel joint and bottom through the materail tube of heat exchanger tube, cooling medium inlet pipe and cooling medium Chu Guan one end are communicated with entrance point and the port of export of heat exchanger tube respectively, the other end stretches in its cavity through hollow shaft sidewall, and is communicated with all the other two paths of three-way swivel joint respectively.
2. continuous cooling crystallizer according to claim 1, is characterized in that, described driving mechanism by motor, the driving-chain that is fixed on driving wheel on motor output shaft, is enclosed within the driven pulley in hollow shaft and connects driving wheel and driven pulley forms.
3. continuous cooling crystallizer according to claim 1, is characterized in that, described crystallization tank top is provided with the bearing support of fixation hollow axle, between described bearing support and hollow shaft, is provided with clutch shaft bearing.
4. continuous cooling crystallizer according to claim 3, is characterized in that, is provided with the second bearing between described hollow shaft and crystallization tank.
5. continuous cooling crystallizer according to claim 1, is characterized in that, between described hollow shaft and crystallization tank, is provided with sealing ring.
6. continuous cooling crystallizer according to claim 1, is characterized in that, described crystallization tank sidewall is provided with observation panel.
7. continuous cooling crystallizer according to claim 1, is characterized in that, described crystallization tank bottom is taper, and bottom connects a vertical material guiding tube.
8. continuous cooling crystallizer according to claim 1, is characterized in that, described heat exchanger tube vertically arranges.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110269347.2A CN102430261B (en) | 2011-09-13 | 2011-09-13 | Continuous cooling crystallizer |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110269347.2A CN102430261B (en) | 2011-09-13 | 2011-09-13 | Continuous cooling crystallizer |
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| CN102430261A CN102430261A (en) | 2012-05-02 |
| CN102430261B true CN102430261B (en) | 2014-01-15 |
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| CN201110269347.2A Expired - Fee Related CN102430261B (en) | 2011-09-13 | 2011-09-13 | Continuous cooling crystallizer |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103801106B (en) * | 2012-11-02 | 2015-11-25 | 中国石油化工集团公司 | A kind of extension type crystallizer |
| CN104028002B (en) * | 2014-07-02 | 2016-04-27 | 岳阳市钾盐科学研究所 | Outer circulation air cooling crystallization process equipment |
| CN104740885B (en) * | 2015-03-12 | 2016-03-30 | 吉首大学 | A kind of device that brine concentration crystallization after vibration is reclaimed |
| CN105854338B (en) * | 2016-05-11 | 2018-03-13 | 南宁市夏阳化工科技有限责任公司 | Produce the tubulation crystallizer of urea for vehicle |
| CN106823445A (en) * | 2017-04-13 | 2017-06-13 | 国家海洋局天津海水淡化与综合利用研究所 | A kind of continuous production Two-way Cycle freezing and crystallizing device |
| CN107281775A (en) * | 2017-08-16 | 2017-10-24 | 广东海翔教育科技有限公司 | A kind of energy-conserving and environment-protective crystallizing tank |
| CN111411305B (en) * | 2020-04-21 | 2021-09-14 | 五矿营口中板有限责任公司 | High-toughness high-Ti low-alloy steel with thick glass lining and good glass lining performance and manufacturing method thereof |
| CN112619198B (en) * | 2020-12-07 | 2022-02-11 | 迈安德集团有限公司 | Cooling crystallization box |
| CN114705872B (en) * | 2022-06-06 | 2022-08-23 | 南京澳林生物科技有限公司 | Anti-crystallization lipoprotein (a) detection kit and use method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2472780Y (en) * | 2001-03-29 | 2002-01-23 | 王修立 | Single pot type one-step process flow ammonium chloride crystallizing device |
| CN2657750Y (en) * | 2003-07-09 | 2004-11-24 | 姜向前 | Cooling crystallization tank |
| CN201543266U (en) * | 2009-09-30 | 2010-08-11 | 安徽丰原化工装备有限公司 | Double-cold crystallizer |
| CN201551868U (en) * | 2009-09-18 | 2010-08-18 | 天津渤海化工有限责任公司天津碱厂 | Ammonium sulfate crystallizer |
-
2011
- 2011-09-13 CN CN201110269347.2A patent/CN102430261B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2472780Y (en) * | 2001-03-29 | 2002-01-23 | 王修立 | Single pot type one-step process flow ammonium chloride crystallizing device |
| CN2657750Y (en) * | 2003-07-09 | 2004-11-24 | 姜向前 | Cooling crystallization tank |
| CN201551868U (en) * | 2009-09-18 | 2010-08-18 | 天津渤海化工有限责任公司天津碱厂 | Ammonium sulfate crystallizer |
| CN201543266U (en) * | 2009-09-30 | 2010-08-11 | 安徽丰原化工装备有限公司 | Double-cold crystallizer |
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| CN102430261A (en) | 2012-05-02 |
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