CN103537115B - A kind of crystallization cooler and method thereof that extends the outer circulation type crystallizer operation cycle - Google Patents
A kind of crystallization cooler and method thereof that extends the outer circulation type crystallizer operation cycle Download PDFInfo
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- CN103537115B CN103537115B CN201310496469.4A CN201310496469A CN103537115B CN 103537115 B CN103537115 B CN 103537115B CN 201310496469 A CN201310496469 A CN 201310496469A CN 103537115 B CN103537115 B CN 103537115B
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Abstract
The invention discloses a kind of crystallization cooler that extends the outer circulation type crystallization process operation cycle. Mainly solve the heat transfer property deterioration, crystallization cooler blocking pipe of crystallization cooler in outer circulation type crystallisation by cooling process, frequently stop and short problem of operation cycle. To mix with fresh feed from recycle stock in crystallizer, and enter evaporator section interior by evaporation working solution cooling down, thereby produce degree of supersaturation, then enter crystallizer crystallization; In evaporator section, the working solution gas phase of evaporation enters condensation segment, gets off and again gets back to evaporator section by gravity with chilled water heat exchange condensation; By control valve and working solution gas phase formation control loop, thereby control the evaporating temperature of working solution by the flow of controlling chilled water, control heat exchange pipe of evaporator internal-external temperature difference and eliminate fouling thereby realize.
Description
Technical field
The invention belongs to chemical technology field, be specifically related to the cooler of outer circulation type crystallization process, outstandingIt is Olso crystallizer, crystallization cooler when the crystallisation by cooling of DTB crystallizer and DP crystallizer andIts method for crystallising.
Background technology
Industrial crystallization is a basic chemical enginnering process, manufactures various products all relevant with crystallization.As inorganic fertilizer, inorganic salts, chemical reagent, petrochemicals and fiery explosive etc. Crystallisation by cooling is doneFor one of significant process of industrial crystallization, reach supersaturation and crystallize out is applicable to molten by coolingXie Du is significantly reduced system with the reduction of temperature.
Partition heat exchange crystallisation by cooling be crystallization mode most widely used in pharmacy and chemical process itOne, common industrial employing outer circulation type crystallisation by cooling. This crystallization mode is by oversaturated generation districtTerritory and crystal growth district are separately positioned on two places of crystallizer, for crystal growth provide one goodCondition, crystal can grow up to crystal greatly and uniformly in crystallizer.
In outer circulation type crystallisation by cooling, oversaturated generation equipment is a crystallization cooler. This is establishedStandby is the key equipment of outer circulation type crystallization, is not only controlling the degree of supersaturation of crystallizer, priorIt is the cycle that is determining the continued operation of crystallizer. In industrial production, crystallization cooler is generally rowChimney cooler, cooling medium is generally the chilled water of 6-10 DEG C. The cooler of this kind of form is due to quiltTemperature difference excessive (temperature difference is the smaller the better) between cooling solution and heat-transfer area, is very easy to crystallization dirt,Not only cause heat transfer property to worsen, affect the control of degree of supersaturation; And cause in severe case coldCondenser stops up, and causes crystallizer to stop. Due to above reason, crystallization cooler is industrial crystallization processThe bottleneck equipment of long period continued operation.
Summary of the invention
The defect or the deficiency that exist for background technology, the object of the invention is to, and provides a kind of and extendCrystallization cooler and the method thereof in outer circulation type crystallizer operation cycle, used this crystallization cooler, adoptsCan eliminate the scale formation of crystallization cooler by the method, control the generation of degree of supersaturation, outside prolongationThe cycle of circulation-type crystallizer continued operation.
In order to realize above-mentioned task, the present invention takes following technical solution:
A crystallization cooler that extends the outer circulation type crystallization process operation cycle, this equipment comprises condensationSection and evaporator section, condensation segment is positioned on evaporator section, is respectively arranged with condenser at the two ends of condensation segmentUpper cover and condenser low head, be respectively arranged with evaporimeter upper cover and evaporation at the two ends of evaporator sectionDevice low head, condenser low head and evaporimeter upper cover is stacked links together; On condenser, sealFirst side is provided with chilled water outlet, and condensation segment one side top is provided with the import of working solution gas phase, condensationIntersegmental part is evenly provided with condenser bundles, and condensation segment bottom one side is provided with working solution liquid-phase outlet,A side at condenser low head is provided with chilled water import, and chilled water import arranges control valve; SteamingOne side of hair device upper cover is set side by side with working solution and supplements mouth and working solution gaseous phase outlet, working solution gasOutlet is connected by pipeline with the import of working solution gas phase mutually, set temperature control instruction and tune on pipelineJoint valve formation control loop, above evaporator section, a side is provided with recycle stock outlet, at the bottom of evaporator sectionPortion's one side is provided with recycle stock import, and a side of evaporimeter low head is provided with the import of working solution liquid phase,The import of working solution liquid phase is connected with the working solution liquid-phase outlet of condensation segment bottom one side setting.
The present invention also has following other technologies feature:
Utilize crystallization cooler as above to carry out crystallization, comprise following technical step:
1) will mix with fresh feed from recycle stock in crystallizer, enter in evaporator section by evaporationThe evaporation working solution cooling down of filling in section, thus degree of supersaturation produced, then enter crystallizer crystallization;
2) in evaporator section, the working solution gas phase of evaporation enters condensation segment, gets off logical with chilled water heat exchange condensationCross gravity and again get back to evaporator section;
3) flow of the control loop control chilled water forming by control valve and temperature control instruction, fromAnd the evaporating temperature of control working solution is controlled heat exchange pipe of evaporator internal-external temperature difference and eliminates knot thereby realizeDirt.
The crystallization cooler in described prolongation outer circulation type crystallization process operation cycle, is characterized in that,In evaporator section B, be filled with working solution, working solution be dimethyl ether, dimethoxym ethane, methyl tertiary butyl ether(MTBE),Diisopropyl ether, ethanol or cold-producing medium R-22 and substitute thereof and two or more mixture thereof.
Described crystallization cooler and method thereof can be used in the crystallization process of piperazine solution, but do not limitIn said process.
The present invention uses the mode crystallization control cooler wall of evaporative condenser and the temperature difference of solution, toolThere is following advantage:
1), by the vaporization and condensation heat exchange of working solution, can, by controlling the operating temperature of working solution, makeObtain crystallization cooler internal-external temperature difference little, eliminate fouling, extend the crystallizer operation cycle;
2) because working solution conducts heat by vaporization and condensation, heat transfer coefficient is large, can reduce heat exchange area,Reduce investment outlay.
Brief description of the drawings
Fig. 1 is crystallization cooler schematic diagram of the present invention.
Mark in accompanying drawing represents respectively:
A condensation segment: comprising: 1, chilled water outlet, 2, the import of working solution gas phase, 3, working solution liquidOutlet mutually, 4, chilled water import, 10, condenser upper cover, 11, condenser bundles, 12, coldCondenser low head, 16, pipeline, 18, control valve, 19, temperature control instruction;
B evaporator section: comprising: 5, working solution supplements mouthful, 6, working solution gaseous phase outlet, 7, recycleMaterial outlet, 8, recycle stock import, 9, the import of working solution liquid phase, 13, evaporimeter upper cover, 14,Evaporimeter tube bank, 15, evaporimeter low head, 17, pipeline.
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Detailed description of the invention
Adopt the crystallization in the prolongation outer circulation type crystallization process operation cycle described in summary of the invention coolingDevice, provides following embodiment according to the technical step described in summary of the invention, the invention is not restricted to theseEmbodiment.
Embodiment 1:
60 DEG C of piperazine solution, by DTB crystallizer crystallisation by cooling under the condition of 20 DEG C, adopt respectivelyTraditional shell and tube cooler and crystallization cooler of the present invention carry out crystallisation by cooling. Traditional shell and tubeCooler is directly by the water quench of 6～10 DEG C. The working solution of crystallization cooler of the present invention is diformazanEther, chilled water temperature is for being 6～10 DEG C. The recycle stock that enters crystallization cooler is 4800kg/h,The piperazine solution of 23 DEG C, the control loop control forming by control valve 18 and temperature control instruction 19The flow of chilled water, thus the evaporating temperature of control working solution is 18 DEG C, and recycle stock is cooled to20 DEG C enter crystallizer.
Traditional shell and tube cooler operation is after 112 hours, and cooler stops up and can not move; The present inventionCrystallization cooler operation after 205 hours, take crystallization cooler apart, have no obvious scale formation.
Embodiment 2:
As described in Example 1, the traditional shell and tube cooler and the crystallization of the present invention that adopt are respectively coldBut device carries out crystallisation by cooling, and 4 Crystallization is identical with embodiment 1 with control mode, differenceBe that working solution of the present invention is dimethoxym ethane.
Traditional shell and tube cooler operation is after 102 hours, and cooler stops up and can not move; The present inventionCrystallization cooler operation after 200 hours, take crystallization cooler apart, have no obvious scale formation.
Embodiment 3:
As described in Example 1, the traditional shell and tube cooler and the crystallization of the present invention that adopt are respectively coldBut device carries out crystallisation by cooling, and 4 Crystallization is identical with embodiment 1 with control mode, differenceBe that working solution of the present invention is methyl tertiary butyl ether(MTBE).
Traditional shell and tube cooler operation is after 95 hours, and cooler stops up and can not move; Of the present inventionThe operation of crystallization cooler, after 200 hours, is taken crystallization cooler apart, has no obvious scale formation.
Embodiment 4:
As described in Example 1, the traditional shell and tube cooler and the crystallization of the present invention that adopt are respectively coldBut device carries out crystallisation by cooling, and 4 Crystallization is identical with embodiment 1 with control mode, differenceBe that working solution of the present invention is diisopropyl ether.
Traditional shell and tube cooler operation is after 90 hours, and cooler stops up and can not move; Of the present inventionThe operation of crystallization cooler, after 200 hours, is taken crystallization cooler apart, has no obvious scale formation.
Embodiment 5:
As described in Example 1, the traditional shell and tube cooler and the crystallization of the present invention that adopt are respectively coldBut device carries out crystallisation by cooling, and 4 Crystallization is identical with embodiment 1 with control mode, differenceBe that working solution of the present invention is ethanol.
Traditional shell and tube cooler operation is after 103 hours, and cooler stops up and can not move; The present inventionCrystallization cooler operation after 200 hours, take crystallization cooler apart, have no obvious scale formation.
Embodiment 6:
As described in Example 1, the traditional shell and tube cooler and the crystallization of the present invention that adopt are respectively coldBut device carries out crystallisation by cooling, and 4 Crystallization is identical with embodiment 1 with control mode, differenceBe that working solution of the present invention is R-22.
Traditional shell and tube cooler operation is after 105 hours, and cooler stops up and can not move; The present inventionCrystallization cooler operation after 200 hours, take crystallization cooler apart, have no obvious scale formation.
Claims (4)
1. extend the crystallization cooler in outer circulation type crystallization process operation cycle, this equipmentComprise condensation segment A and evaporator section B, it is characterized in that: condensation segment A is positioned on evaporator section B,Be respectively arranged with condenser upper cover (10) and condenser low head at the two ends of condensation segment(12), be respectively arranged with evaporimeter upper cover (13) and evaporimeter at the two ends of evaporator section BLow head (15), condenser low head (12) and the stacked company of evaporimeter upper cover (13)Be connected together; Be provided with chilled water outlet (1) in condenser upper cover (10) one sides, coldSolidifying section A mono-side top is provided with working solution gas phase import (2), and condensation segment A is inner evenly to be arrangedHave condenser bundles (11), condensation segment A bottom one side is provided with working solution liquid-phase outlet (3),A side at condenser low head (12) is provided with chilled water import, and chilled water import arranges tuneJoint valve (18); Being set side by side with working solution in a side of evaporimeter upper cover (13) supplementsMouth (5) and working solution gaseous phase outlet (6), working solution gaseous phase outlet (6) and working solution gasPhase import (2) is connected by pipeline (16), and the upper set temperature control of pipeline (16) refers toShow (19) and control valve (18) formation control loop, above evaporator section B, a side is provided withRecycle stock outlet (7), in evaporator section B bottom, one side is provided with recycle stock import (8),One side of evaporimeter low head (15) is provided with working solution liquid phase import (9), working solution liquidPhase import (9) is connected with the working solution liquid-phase outlet (3) that condensation segment A bottom one side arranges;In described evaporator section B, be filled with working solution, working solution is dimethyl ether, dimethoxym ethane, methyl-tertButyl ether, diisopropyl ether, ethanol or cold-producing medium R-22 and two or more mixing thereofThing.
2. utilize the crystallization in the prolongation outer circulation type crystallization process operation cycle described in claim 1The method of cooler crystallization, is characterized in that, comprises following technical step:
1) will mix with fresh feed from recycle stock in crystallizer, enter in evaporator section BBy the evaporation working solution cooling down of filling in evaporator section B, thereby produce degree of supersaturation,Enter again crystallizer crystallization;
2) in evaporator section, the working solution gas phase of evaporation enters condensation segment, with chilled water heat exchange condensationGet off and again get back to evaporator section by gravity;
3) the control loop control forming by control valve (18) and temperature control instruction (19)The flow of chilled water processed, thereby the evaporating temperature of control working solution, and then realize and control evaporimeterHeat exchanger tube internal-external temperature difference and eliminate fouling.
3. method as claimed in claim 2, is characterized in that, described crystallizer isOlso crystallizer, DTB crystallizer, DP crystallizer or other produce by outer circulation modeThe crystallizer of raw degree of supersaturation.
4. method as claimed in claim 2, is characterized in that, described crystallization coolerFor the crystallization process of piperazine solution.
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| CN201310496469.4A CN103537115B (en) | 2013-10-21 | 2013-10-21 | A kind of crystallization cooler and method thereof that extends the outer circulation type crystallizer operation cycle |
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| CN103537115B true CN103537115B (en) | 2016-05-25 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6077438A (en) * | 1998-12-22 | 2000-06-20 | Combichem, Inc. | Automated on-line evaporation light scattering detection to quantify isolated fluid sample compounds in microtiter plate format |
| CN101077518A (en) * | 2007-06-29 | 2007-11-28 | 重庆大学 | Hot pipe type continuous casting crystallizer |
| CN102992409A (en) * | 2012-12-20 | 2013-03-27 | 中冶赛迪工程技术股份有限公司 | Ferrous sulfate solution refrigerating crystallization device and method |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102580347B (en) * | 2012-03-02 | 2014-08-27 | 浙江金科日化原料有限公司 | Continuous crystallization method of tetraacetylethylenediamine |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6077438A (en) * | 1998-12-22 | 2000-06-20 | Combichem, Inc. | Automated on-line evaporation light scattering detection to quantify isolated fluid sample compounds in microtiter plate format |
| CN101077518A (en) * | 2007-06-29 | 2007-11-28 | 重庆大学 | Hot pipe type continuous casting crystallizer |
| CN102992409A (en) * | 2012-12-20 | 2013-03-27 | 中冶赛迪工程技术股份有限公司 | Ferrous sulfate solution refrigerating crystallization device and method |
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