CN103537115A - Crystallization cooler capable of prolonging operation period of external circulating type crystallizer and method thereof - Google Patents
Crystallization cooler capable of prolonging operation period of external circulating type crystallizer and method thereof Download PDFInfo
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- CN103537115A CN103537115A CN201310496469.4A CN201310496469A CN103537115A CN 103537115 A CN103537115 A CN 103537115A CN 201310496469 A CN201310496469 A CN 201310496469A CN 103537115 A CN103537115 A CN 103537115A
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Abstract
The invention discloses a crystallization cooler capable of prolonging the operation period of external circulating type crystallization. The crystallization cooler mainly solves the problems of a conventional crystallization cooler that in an external circulating type cooling and crystallization process, heat transfer performance deteriorates, a pipeline is plugged to cause frequent faults and the operation period is short. Circulating materials in a crystallizer are mixed with fresh feeding materials, and the mixture is cooled in an evaporation section by evaporating working liquid to generate the degree of supersaturation, and then is crystallized in the crystallizer; the gas phase of the working liquid evaporated in the evaporation section enters a condensation section, exchanges heat with frozen water to be condensed and then flows back to the evaporation section through gravity; a control loop is formed by the working liquid gas phase and a regulating valve, the evaporation temperature of the working liquid can be controlled by controlling the flow rate of chilled water, thus controlling the difference of temperatures inside and outside a heat exchange pipe of the evaporator and further preventing scaling.
Description
Technical field
The invention belongs to chemical technology field, be specifically related to the cooler of outer circulation type crystallization process, Olso crystallizer especially, DTB crystallizer and DP crystallizer crystallization cooler and the method for crystallising thereof during for crystallisation by cooling.
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, as one of significant process of industrial crystallization, reaches supersaturation and crystallize out by cooling, is applicable to the reduction of solubility with temperature and significantly reduced system.
Partition heat exchange crystallisation by cooling is one of crystallization mode most widely used in pharmacy and chemical process, common industrial employing outer circulation type crystallisation by cooling.This crystallization mode is separately positioned on oversaturated generation region and crystal growth district at two places of crystallizer, for crystal growth provides a good condition, crystal, can in crystallizer, grow up to crystal greatly and uniformly.
In outer circulation type crystallisation by cooling, oversaturated generation equipment is a crystallization cooler.This equipment is the key equipment of outer circulation type crystallization, is not only controlling the degree of supersaturation of crystallizer, the more important thing is the cycle of the continued operation that is determining crystallizer.In industrial production, crystallization cooler is generally shell and tube cooler, and cooling medium is generally the chilled water of 6-10 ℃.The cooler of this kind of form, due to the temperature difference being cooled between solution and heat-transfer area excessive (temperature difference is the smaller the better), is very easy to crystallization dirt, not only causes heat transfer property to worsen, and affects the control of degree of supersaturation; And cause in severe case blockage of condenser, cause crystallizer to stop.Due to above reason, crystallization cooler is the bottleneck equipment of industrial crystallization process long period continued operation.
Summary of the invention
The defect or the deficiency that for background technology, exist, the object of the invention is to, a kind of crystallization cooler and method thereof that extends the outer circulation type crystallizer operation cycle is provided, use this crystallization cooler, adopt the method can eliminate the scale formation of crystallization cooler, control the generation of degree of supersaturation, extend the cycle of outer circulation type crystallizer continued operation.
In order to realize above-mentioned task, the present invention takes following technical solution:
A kind of crystallization cooler that extends the outer circulation type crystallization process operation cycle, this equipment comprises condensation segment and evaporator section, condensation segment is positioned on evaporator section, at the two ends of condensation segment, be respectively arranged with condenser upper cover and condenser low head, at the two ends of evaporator section, be respectively arranged with evaporimeter upper cover and evaporimeter low head, condenser low head and evaporimeter upper cover is stacked links together; In condenser upper cover one side, be provided with chilled water outlet, condensation segment one side top is provided with the import of working solution gas phase, condensation segment inside is evenly provided with condenser bundles, 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; A side at evaporimeter upper cover is set side by side with supplementary mouthful of working solution and working solution gaseous phase outlet, working solution gaseous phase outlet and the import of working solution gas phase are connected by pipeline, on pipeline, set temperature is controlled indication and control valve formation control loop, above evaporator section, a side is provided with recycle stock outlet, in evaporator section bottom, one side is provided with recycle stock import, one side of evaporimeter low head is provided with the import of working solution liquid phase, and 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 the evaporation working solution cooling down of passing through filling in evaporator section in evaporator section, thereby produce degree of supersaturation, then enter crystallizer crystallization;
2) 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;
3) control loop forming by control valve and temperature control indication is controlled the flow of chilled water, thereby controls the evaporating temperature of working solution, thereby realization is controlled heat exchange pipe of evaporator internal-external temperature difference and eliminated fouling.
The crystallization cooler in described prolongation outer circulation type crystallization process operation cycle, it is characterized in that, in evaporator section B, be filled with working solution, working solution is dimethyl ether, dimethoxym ethane, methyl tertiary butyl ether(MTBE), diisopropyl ether, ethanol or cold-producing medium R-22 and substitute and two or more mixture thereof.
Described crystallization cooler and method thereof can be used in the crystallization process of piperazine solution, but are not limited to said process.
The present invention uses the mode crystallization control cooler wall of evaporative condenser and the temperature difference of solution, has the following advantages:
1) by the vaporization and condensation heat exchange of working solution, can make crystallization cooler internal-external temperature difference little by controlling the operating temperature of working solution, 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, reduces investment outlay.
Accompanying drawing explanation
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 liquid-phase outlet, 4, chilled water import; 10, condenser upper cover, 11, condenser bundles, 12, condenser low head; 16, pipeline, 18, control valve, 19, temperature controls indication;
B evaporator section: comprising: 5, working solution supplements mouthful, 6, working solution gaseous phase outlet, 7, recycle stock 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.
The specific embodiment
The crystallization cooler that adopts the prolongation outer circulation type crystallization process operation cycle described in summary of the invention, provides following embodiment according to the technical step described in summary of the invention, the invention is not restricted to these embodiment.
Embodiment 1:
60 ℃ of piperazine solution are by DTB crystallizer crystallisation by cooling under the condition of 20 ℃, and the traditional shell and tube cooler and the crystallization cooler of the present invention that adopt respectively carry out crystallisation by cooling.Traditional shell and tube cooler is directly by the water quench of 6～10 ℃.The working solution of crystallization cooler of the present invention is dimethyl ether, and chilled water temperature is for being 6～10 ℃.The recycle stock that enters crystallization cooler is 4800kg/h, the piperazine solution of 23 ℃, by control valve 18 and temperature, control the flow of the control loops control chilled waters of indication 19 formation, thereby the evaporating temperature of control working solution is 18 ℃, makes recycle stock be cooled to 20 ℃ to enter crystallizer.
Traditional shell and tube cooler operation is after 112 hours, and cooler stops up and can not move; Crystallization cooler operation of the present invention, after 205 hours, is taken crystallization cooler apart, has no obvious scale formation.
Embodiment 2:
As described in Example 1, the traditional shell and tube cooler and the crystallization cooler of the present invention that adopt respectively carry out crystallisation by cooling, and 4 Crystallization is identical with embodiment 1 with control mode, and difference is 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; Crystallization cooler operation of the present invention, after 200 hours, is taken crystallization cooler apart, has no obvious scale formation.
Embodiment 3:
As described in Example 1, the traditional shell and tube cooler and the crystallization cooler of the present invention that adopt respectively carry out crystallisation by cooling, and 4 Crystallization is identical with embodiment 1 with control mode, and difference is 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; Crystallization cooler operation of the present invention, 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 cooler of the present invention that adopt respectively carry out crystallisation by cooling, and 4 Crystallization is identical with embodiment 1 with control mode, and difference is 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; Crystallization cooler operation of the present invention, 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 cooler of the present invention that adopt respectively carry out crystallisation by cooling, and 4 Crystallization is identical with embodiment 1 with control mode, and difference is 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; Crystallization cooler operation of the present invention, after 200 hours, is taken crystallization cooler apart, has no obvious scale formation.
Embodiment 6:
As described in Example 1, the traditional shell and tube cooler and the crystallization cooler of the present invention that adopt respectively carry out crystallisation by cooling, and 4 Crystallization is identical with embodiment 1 with control mode, and difference is 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; Crystallization cooler operation of the present invention, after 200 hours, is taken crystallization cooler apart, has no obvious scale formation.
Claims (5)
1. a crystallization cooler that extends the outer circulation type crystallization process operation cycle, this equipment comprises condensation segment A and evaporator section B, it is characterized in that: condensation segment A is positioned on evaporator section B, at the two ends of condensation segment, be respectively arranged with condenser upper cover (10) and condenser low head (12), at the two ends of evaporator section B, be respectively arranged with evaporimeter upper cover (13) and evaporimeter low head (15), condenser low head (12) and stacked the linking together of evaporimeter upper cover (13), in condenser upper cover (10) one sides, be provided with chilled water outlet (1), condensation segment A mono-side top is provided with working solution gas phase import (2), condensation segment A inside is evenly provided with 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 control valve (18), a side at evaporimeter upper cover (13) is set side by side with working solution supplementary mouthful (5) and a working solution gaseous phase outlet (6), working solution gaseous phase outlet (6) is connected by pipeline (16) with working solution gas phase import (2), the upper set temperature of pipeline (16) is controlled indication (19) and control valve (18) formation control loop, above evaporator section B, a side is provided with recycle 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 liquid phase import (9) is connected with the working solution liquid-phase outlet (3) that condensation segment A bottom one side arranges.
2. the crystallization cooling means of utilizing the prolongation outer circulation type crystallization process operation cycle described in claim 1, is characterized in that, comprises following technical step:
1) will mix with fresh feed from recycle stock in crystallizer, enter the evaporation working solution cooling down of passing through filling in evaporator section B in evaporator section B, thereby produce degree of supersaturation, then enter crystallizer crystallization;
2) 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;
3) control loop forming by control valve (18) and temperature control indication (19) is controlled the flow of chilled water, thereby controls the evaporating temperature of working solution, and then realization is controlled heat exchange pipe of evaporator internal-external temperature difference and eliminated fouling.
3. the crystallization cooler in prolongation outer circulation type crystallization process operation cycle as claimed in claim 1, it is characterized in that, in evaporator section B, be filled with working solution, working solution is dimethyl ether, dimethoxym ethane, methyl tertiary butyl ether(MTBE), diisopropyl ether, ethanol or cold-producing medium R-22 and substitute and two or more mixture thereof.
4. method as claimed in claim 2, is characterized in that, described crystallizer is Olso crystallizer, DTB crystallizer, and DP crystallizer or other produce the crystallizer of degree of supersaturation by outer circulation mode.
5. method as claimed in claim 2, is characterized in that, crystallization cooler described above is for the crystallization process of piperazine solution.
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| Application Number | Priority Date | Filing Date | Title |
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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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| 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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| CN103537115A true CN103537115A (en) | 2014-01-29 |
| CN103537115B CN103537115B (en) | 2016-05-25 |
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Citations (4)
| 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 |
| CN102580347A (en) * | 2012-03-02 | 2012-07-18 | 浙江金科日化原料有限公司 | Continuous crystallization method of tetraacetylethylenediamine |
| 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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2013
- 2013-10-21 CN CN201310496469.4A patent/CN103537115B/en active Active
Patent Citations (4)
| 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 |
| CN102580347A (en) * | 2012-03-02 | 2012-07-18 | 浙江金科日化原料有限公司 | Continuous crystallization method of tetraacetylethylenediamine |
| 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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