CN202237354U - Melting crystallizer - Google Patents

Melting crystallizer Download PDF

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Publication number
CN202237354U
CN202237354U CN2011203778280U CN201120377828U CN202237354U CN 202237354 U CN202237354 U CN 202237354U CN 2011203778280 U CN2011203778280 U CN 2011203778280U CN 201120377828 U CN201120377828 U CN 201120377828U CN 202237354 U CN202237354 U CN 202237354U
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China
Prior art keywords
crystallizer
cooling medium
film
crystallization
mozzle
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Expired - Lifetime
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CN2011203778280U
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卢咏琰
肖剑
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China Petroleum and Chemical Corp
Sinopec Shanghai Research Institute of Petrochemical Technology
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China Petroleum and Chemical Corp
Sinopec Shanghai Research Institute of Petrochemical Technology
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Abstract

The utility model relates to a melting crystallizer, which mainly solves the problem that melting crystallizers have complicated structures and are difficultly industrialized in the prior art. The melting crystallizer comprises a columnar shell, wherein opposite ends of the shell are enclosed by a top plate and a lower head; a plurality of vertical falling film crystallization tubes are arranged in the shell of the crystallizer; a crystallization tube bundle is fixed through an upper tube plate and a lower tube plate; the upper part of the crystallizer is provided with a material inlet and a material overflow port; the lower head of the crystallizer is provided with a material outlet; a guide tube is inserted in each falling film crystallization tube; a diameter ratio of the guide tube and the falling film crystallization tubes is 0.05-0.98; and the upper part of the guide tube is provided with a vent and the lower end of the guide tube is provided with a guide component. By the technical scheme, the problem is better solved; and the melting crystallizer can be used for industrial production of crystallization.

Description

Melting crystallizer
Technical field
The utility model relates to a kind of melting crystallizer.
Background technology
Along with the development of chemical industry, increasingly high for the purity requirement of polymer monomer and raw material.And these monomers exist with the form of admixture of isomeric compound usually, for isomer and thermal sensitivity system, because of boiling point problem and thermal sensitivity problem, if employing distillation technology, often tens or up to a hundred blocks column plates of needs and high reflux ratio and decompression operation.Operating condition is harsh, and is higher to equipment material and requirement on machining accuracy.Even so, the charing in the rectifying still, coking, phenomenons such as polymerization can't be avoided, and product yield is lower, also can't obtain high purity product.The fusion-crystallization technology can be avoided these problems, and for these systems, the fusing point of material often can differ tens degree, can use the fusion-crystallization technical point to leave.
The fusion-crystallization technology mainly contains suspension crystallization technology and film-falling crystallization technology.In the suspension crystallization technology, the crystal that obtains in the crystallizer need be transported to and be further purified separation in the scrubbing tower.The one side of this technology relates to solid-liquid and carries, and solid is prone to stop up in pipeline, and crystal needs scrubbing tower washing purifying, complex equipments on the other hand.In the existing film-falling crystallization technology; Through after crystallization, the sweating, directly melt crystal and can obtain high purity product, but its device structure is complicated in the liquid material entering crystallizer; Operating condition is harsh; Existing simultaneously film-falling crystallization device when amplifying, elongated along with crystallizer, crystal is easy to collapse on crystallizer.
Chinese patent CN1090514C has introduced a kind of method and apparatus through fractional crystallization separate substance from liquid mixture, and its fusion through crystallization technique and heat pump techniques has improved capacity usage ratio.But not enough below this device exists: every crystallizer of this device carries out crystallization through the evaporation of the cooling medium in the crystallizer with the separate substance heat exchange; This just makes; Every crystallizer of one side must bear the evaporating pressure of cooling medium; On the other hand, with regard to the applied cooling medium that can volatilize in the present industry, often equipment had corrosivity.More than two aspects all the processing and the Material Selection of equipment are had high requirement, equipment manufacturing cost and maintenance cost are higher.Crystal is grown at the crystallizer outer wall equipment capacity is restricted.For improving the crystal production ability, in the crystallizer crystallizer as much as possible need be set, but this device; Crystal is grown in the crystallizer outside; For leaving the space to crystal growth, just need leave enough spaces between crystallizer, promptly need reduce the quantity of crystallizer; The existence of above contradiction is restricted the production capacity of this crystallizer, is unfavorable for the amplification of crystallizer.Crystal is grown on the crystallizer outer wall, and for large-scale crystallizer, crystallizer is longer, the easy phenomenon that collapses of crystal.
Summary of the invention
The utility model will solve existing melting crystallizer complex equipments, and being unfavorable for the technical problem of amplifying provides a kind of novel melting crystallizer, and this device has simple in structure, is easy to the advantage that industry is amplified.
For solving the problems of the technologies described above, the utility model adopts following technical scheme: a kind of melting crystallizer 1 comprises vertically arranged film-falling crystallization pipe 5 and cooling medium distribution tray 10 in cylindrical outer cover 2, the shell 2; Shell 2 is through top board 3 and low head 15 sealing in the opposite end, and shell 2 tops are provided with cooling medium inlet 17, material inlet 6 and material overfall 7, and the bottom is provided with cooling medium outlet 13, and crystallizer low head 15 is provided with material outlet 14; Film-falling crystallization pipe 5 is fixing with lower perforated plate 9 through upper perforated plate 8, all is inserted with mozzle 4 on the film-falling crystallization pipe 5, and mozzle 4 tops are provided with steam vent 20, and the lower end is provided with guiding subassembly 21; Arrangement position corresponding to crystallizer on the cooling medium distribution tray 10 is provided with cooling medium pod apertures 16, downflow weir 11, downspout 12 and cooling medium guiding subassembly 19, and film-falling crystallization pipe 5 passes pod apertures 16.
In the technique scheme, the diameter of mozzle 4 and film-falling crystallization pipe 5 than preferable range is between 0.05~0.98; The diameter of pod apertures 16 and crystallizer 5 is 0.05~0.98 than preferable range; Mozzle 4 has inner member 18 with the lower part in the crystallizer 5, and this inner member of optimized technical scheme is the fin of complete or perforate; Guiding subassembly 21 on the optimized technical scheme mozzle is to become 5 °~85 ° deflector with level; Optimized technical scheme cooling medium guiding subassembly 19 is to become 5 °~85 ° deflector with level; The number preferable range of downflow weir 11 is 1~50; The number preferable range of downspout 12 is 1~50.
Owing to adopted technique scheme; This crystallizer can be selected the characteristics according to separation of material for use, selects multiple cooling medium for use, as selecting water as cooling medium in the dichloro-benzenes crystallization process; The mixture that can select ethylene glycol and water in the xylenes crystallization process is as cooling medium; Crystallizer can be by non-pressure vessel processing design, and cooling medium is low to equipment corrosion, effectively reduces the cost and the maintenance cost of equipment; Cooling medium forms thin liquid film on the crystallizer outer wall, cooling medium needn't be full of crystallizer, has practiced thrift cooling medium, and the weight when having reduced the equipment operation simultaneously helps equipment enlarging; Cooling medium and material have been realized in the same way and have been flowed heat exchange; Because and flow heat exchange and reduced the temperature difference between separation of material and cooling medium, reduced degree of supersaturation, reduced the speed of growth of crystal; Reduced impurity and contained, more helped crystallization process and carry out intracrystalline; Fin is housed in the crystallizer, and fin can effectively support crystal on the one hand, prevents that crystal from collapsing, and has strengthened the heat transfer between crystal and cooling medium on the other hand, can reduce the time of sweating in the crystallization process; Device structure is simple, is easy to amplify.Through above experimental provision mixed xylenes is carried out Crystallization Separation; Paraxylene mass concentration 80% in the mixed xylenes charging, Affecting Ortho-Xylene's Quality concentration 2%, meta-xylene 10%; Ethylbenzene 8% finally can obtain mass concentration and be higher than 99.8% paraxylene product.
Description of drawings
Fig. 1 film-falling crystallization device sketch map.
Among Fig. 1,1 is falling-film crystallizer, and 2 is shell, and 3 is top board, and 4 is mozzle; 5 is crystallizer, and 6 is material inlet, and 7 is the material overfall, and 8 is upper perforated plate, and 9 is lower perforated plate; 10 is the cooling medium distribution tray, and 11 is downflow weir, and 12 is downspout, and 13 are the cooling medium outlet; 14 is material outlet, and 15 is low head, and 17 is cooling medium inlet, and 20 is steam vent.
Pipe and tower tray sketch map in Fig. 2 falling-film crystallizer;
Among Fig. 2,4 is mozzle, and 5 is crystallizer, and 10 is the cooling medium distribution tray, and 16 is the cooling medium pod apertures, and 18 is inner member, and 19 is the cooling medium guiding subassembly, and 20 is steam vent, and 21 is guiding subassembly.
Fig. 3 film-falling crystallization pipe inner member sketch map;
Fig. 4 crystallizer coolant distribution tower tray sketch map;
Fig. 5 fin structure sketch map;
Among Fig. 5,22 is complete fin,
Fig. 6 fin structure sketch map;
Among Fig. 6,23 is fin with holes.
Through specific embodiment the utility model is further described below, still, the scope of the utility model has more than and is limited to the scope that embodiment covers.
The specific embodiment
[embodiment 1]
The film-falling crystallization device 1 that the utility model proposes is seen Fig. 1, comprises cylindrical outer cover 2, and through top board 3 and low head 15 sealing in the opposite end, top board 3 and low head 15 are fixed on the opposite end through flange; Be provided with many vertically arranged film-falling crystallization pipes 5 in the crystallizer shell; The crystallization tube bank is welded on upper perforated plate 8 and the lower perforated plate 9 fixing; Crystallizer is provided with material inlet 6 and material overfall 7; The crystallizer low head is provided with material outlet 14, and every film-falling crystallization Guan Shangjun is inserted with mozzle 4, and mozzle 4 compares 0.05~0.98 with the diameter of film-falling crystallization pipe 5; Mozzle top is provided with steam vent 20, and the lower end is provided with guiding subassembly 21, sees Fig. 2.The crystallizer shell upper is provided with cooling medium inlet 17, and the bottom is provided with cooling medium outlet 13.Be provided with polylith cooling medium distribution tray 10 in the crystallizer; Arrangement position according to the crystallization tube bank on the cooling medium distribution tray 10 has cooling medium pod apertures 16; Referring to Fig. 4; Crystallizer 5 passes pod apertures, and the diameter of pod apertures 16 and crystallizer 5 is provided with downflow weir 11, downspout 12 than on cooling medium distribution tray between 0.05~0.98, and the cooling medium distribution tray is provided with cooling medium guiding subassembly 19.Referring to Fig. 2 and Fig. 4, the cooling medium distribution tray is provided with downflow weir 11 and downspout 12.Mozzle 4 has inner member 18 with the lower part in the Crystallizer tube 5, and inner member can be complete fin 22, also can be the fin 23 of perforate, referring to Fig. 2, Fig. 3, Fig. 5.Guiding subassembly 21 on the material diversion pipe is to become 5 °~80 ° deflector with level.Cooling medium guiding subassembly guiding subassembly 19 is to become 5 °~85 ° deflector with level.Tower tray is provided with one or more downflow weirs and one or more downspouts, and the crystallization tube bank in the crystallizer can adopt equilateral triangle to arrange, and referring to Fig. 4, tube bank also can be adopted square arrangement.
The Crystallization Separation that is used for the melting crystallizer of the utility model the high-purity paraxylene of mixed xylenes.
Paraxylene mass concentration 80% in the mixed xylenes charging, Affecting Ortho-Xylene's Quality concentration 2%, meta-xylene 10%, ethylbenzene 8%.
The melting crystallizer whole operation process comprises crystallization, sweating, three steps of crystals melt:
6 ℃ of mixed xylenes; With the charging rate of 500L/h, get into the crystallizer top through material inlet 6, the slit that mixed xylenes process mozzle 4 and film-falling crystallization pipe are 5; Through guiding subassembly 21 drainages; On the film-falling crystallization inside pipe wall, form the material liquid film, flow into crystallizer 5, unnecessary mixed xylenes flows out through material overfall 7.-20 ℃ of cooling mediums get into crystallizer through cooling medium inlet 17; Through the cooling medium guiding subassembly 19 on the cooling medium distribution tray 10; Flow into cooling medium pod apertures 16, cooling medium forms the cooling medium liquid film on the outer wall of film-falling crystallization pipe 5, and cooling medium distribution tray 10 is provided with downflow weir 11 and downspout 12; Through the flow of height control cooling medium on every crystallizer of downflow weir, unnecessary cooling medium flows to the next stage tower tray through downspout.Cooling medium liquid film and material liquid film to be purified are realized on the crystallizer wall and the stream heat exchange through above structural design.The mixed xylenes liquid film is along with the crystallizer inwall that is reduced in of temperature is separated out the paraxylene crystal, and uncrystallized raffinate is discharged from bottoms material outlet 14.
After the charging 2 hours; Stop charging; Make cooling medium be elevated to 13 ℃ by certain heating schedule, the temperature of rising crystallizer outer wall cooling medium is carried out the sweating operation, and the purpose of sweating is to contain at the impure liquid of paraxylene crystals with the surface in order to make; In crystal layer, melt, be further purified crystal.The raffinate that sweating obtains is discharged from bottoms material outlet 14.Because the crystallizer inwall is provided with fin, have supporting role for crystal layer on the one hand, prevented that effectively crystal layer from collapsing in the sweating process; Inner fin has played augmentation of heat transfer on the other hand, reduces the effect of sweating time.
Behind the sweating EO, make coolant temperature be elevated to 15 ℃, crystal is melted, obtain high purity product, high purity product is discharged from material outlet 14 and is collected.Finally can obtain mass concentration 99.8% paraxylene product.
[embodiment 2]
The Crystallization Separation that is used for the melting crystallizer of embodiment 1 the high-purity paracide of mixed dichlorobenzene.
Paracide mass concentration 88% in the mixed dichlorobenzene charging, o-dichlorohenzene mass concentration 11.5%, an o-dichlorohenzene 0.5%.
The melting crystallizer whole operation process comprises crystallization, sweating, three steps of crystals melt:
60 ℃ of mixed dichlorobenzenes; Charging rate with 1000L/h gets into the crystallizer top through material inlet 6; The slit that mixed dichlorobenzene process mozzle 4 and film-falling crystallization pipe are 5 through guiding subassembly 21 drainages, forms the material liquid film on the film-falling crystallization inside pipe wall; Flow into crystallizer 5, unnecessary mixed dichlorobenzene flows out through material overfall 7.10 ℃ of cooling mediums get into crystallizer through cooling medium inlet 17; Through the cooling medium guiding subassembly 19 on the cooling medium distribution tray 10; Flow into cooling medium pod apertures 16, cooling medium forms the cooling medium liquid film on the outer wall of film-falling crystallization pipe 5, and cooling medium distribution tray 10 is provided with downflow weir 11 and downspout 12; Through the flow of height control cooling medium on every crystallizer of downflow weir, unnecessary cooling medium flows to the next stage tower tray through downspout.Cooling medium liquid film and material liquid film to be purified are realized on the crystallizer wall and the stream heat exchange through above structural design.The mixed dichlorobenzene liquid film is along with the crystallizer inwall that is reduced in of temperature is separated out the paracide crystal, and uncrystallized raffinate is discharged from bottoms material outlet 14.
After the charging 1 hour; Make cooling medium be elevated to 53 ℃ by certain heating schedule, the temperature of rising crystallizer outer wall cooling medium is carried out the sweating operation, and the purpose of sweating is to contain at the impure liquid of paracide crystals with the surface in order to make; In crystal layer, melt, be further purified crystal.The raffinate that sweating obtains is discharged from bottoms material outlet 14.Because the crystallizer inwall is provided with fin, have supporting role for crystal layer on the one hand, prevented that effectively crystal layer from collapsing in the sweating process; Inner fin has played augmentation of heat transfer on the other hand, reduces the effect of sweating time.
Behind the sweating EO, make coolant temperature be elevated to 70 ℃, crystal is melted, obtain high purity product, high purity product is discharged from material outlet 14 and is collected.Finally can obtain mass concentration 99.5% paracide product.

Claims (8)

1. a melting crystallizer (1) comprises vertically arranged film-falling crystallization pipe (5) and cooling medium distribution tray (10) in cylindrical outer cover (2), the shell (2); Shell (2) seals in the opposite end through top board (3) and low head (15); Shell (2) top is provided with cooling medium inlet (17), material inlet (6) and material overfall (7); The bottom is provided with cooling medium outlet (13), and crystallizer low head (15) is provided with material outlet (14); Film-falling crystallization pipe (5) is fixing through upper perforated plate (8) and lower perforated plate (9), all is inserted with mozzle (4) on the film-falling crystallization pipe (5), and mozzle (4) top is provided with steam vent (20), and the lower end is provided with guiding subassembly (21); The arrangement position that cooling medium distribution tray (10) goes up corresponding to crystallizer is provided with cooling medium pod apertures (16), downflow weir (11), downspout (12) and cooling medium guiding subassembly (19), and film-falling crystallization pipe (5) passes pod apertures (16).
2. the described melting crystallizer of claim 1 is characterized in that the mozzle (4) and the diameter ratio of film-falling crystallization pipe (5) are 0.05~0.98.
3. the described melting crystallizer of claim 1 is characterized in that the diameter ratio of pod apertures (16) and crystallizer (5) is 0.05~0.98.
4. the described melting crystallizer of claim 1 is characterized in that the interior mozzle of crystallizer (5) (4) has inner member (18) with the lower part, and this inner member is the fin (22) of complete or perforate.
5. the described melting crystallizer of claim 1 is characterized in that the guiding subassembly (21) on the mozzle is to become 5 °~85 ° deflector with level.
6. the described melting crystallizer of claim 1 is characterized in that cooling medium guiding subassembly (19) is to become 5 °~85 ° deflector with level.
7. the described melting crystallizer of claim 1, the number that it is characterized in that downflow weir (11) is 1~50.
8. the described melting crystallizer of claim 1, the number that it is characterized in that downspout (12) is 1~50.
CN2011203778280U 2011-09-29 2011-09-29 Melting crystallizer Expired - Lifetime CN202237354U (en)

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Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103086329A (en) * 2013-02-04 2013-05-08 瓮福(集团)有限责任公司 Method for producing electronic-grade sulfuric acid through falling film crystallization
CN103694105A (en) * 2014-01-13 2014-04-02 南通奥凯生物技术开发有限公司 Method for purifying sorbic acid
CN103772137A (en) * 2012-10-25 2014-05-07 中国石油化工股份有限公司 Purification method of p-dichlorobenzene
CN103819435A (en) * 2014-02-17 2014-05-28 扬州大学 Method for separating 3-chlorophthalic anhydride from monochlorophthalic anhydride isomer mixture
CN105013206A (en) * 2014-04-24 2015-11-04 天津东大化工集团有限公司 Melted benzoic acid column for producing high-purity benzoic acid
CN105142748A (en) * 2013-01-22 2015-12-09 Aaa水技术公司 Crystallization system and method
CN105771306A (en) * 2016-05-13 2016-07-20 湖北东方化工有限公司 Static melt crystallizer for purifying and separating material
CN109621478A (en) * 2019-01-25 2019-04-16 孙志良 One kind being used for material purification & isolation static state melting crystallizer
CN112521363A (en) * 2019-09-19 2021-03-19 中国石油化工股份有限公司 Crystallization and purification device and method for ethylene carbonate
CN112569629A (en) * 2015-03-31 2021-03-30 北京普利玛科技有限责任公司 Melt crystallizer
CN112675568A (en) * 2019-10-18 2021-04-20 中国石油化工股份有限公司 Separation and purification device and separation and purification method
CN113893569A (en) * 2020-07-07 2022-01-07 中国石油化工股份有限公司 Static crystallization apparatus and static crystallization method
CN114015416A (en) * 2021-11-27 2022-02-08 浙江皇星化工股份有限公司 Production method of high latent heat energy storage material
CN115177969A (en) * 2021-04-02 2022-10-14 中国石化工程建设有限公司 System and method for separating ethylbenzene from C8 aromatic hydrocarbon
CN115999316A (en) * 2021-10-21 2023-04-25 中国石油化工股份有限公司 Absorption stabilization process and absorption desorption coupling tower thereof

Cited By (20)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103772137A (en) * 2012-10-25 2014-05-07 中国石油化工股份有限公司 Purification method of p-dichlorobenzene
CN105142748A (en) * 2013-01-22 2015-12-09 Aaa水技术公司 Crystallization system and method
CN103086329A (en) * 2013-02-04 2013-05-08 瓮福(集团)有限责任公司 Method for producing electronic-grade sulfuric acid through falling film crystallization
CN103694105A (en) * 2014-01-13 2014-04-02 南通奥凯生物技术开发有限公司 Method for purifying sorbic acid
CN103694105B (en) * 2014-01-13 2015-09-30 南通奥凯生物技术开发有限公司 A kind of method of Sorbic Acid of purifying
CN103819435A (en) * 2014-02-17 2014-05-28 扬州大学 Method for separating 3-chlorophthalic anhydride from monochlorophthalic anhydride isomer mixture
CN105013206A (en) * 2014-04-24 2015-11-04 天津东大化工集团有限公司 Melted benzoic acid column for producing high-purity benzoic acid
CN112569629A (en) * 2015-03-31 2021-03-30 北京普利玛科技有限责任公司 Melt crystallizer
CN105771306A (en) * 2016-05-13 2016-07-20 湖北东方化工有限公司 Static melt crystallizer for purifying and separating material
CN109621478A (en) * 2019-01-25 2019-04-16 孙志良 One kind being used for material purification & isolation static state melting crystallizer
CN112521363A (en) * 2019-09-19 2021-03-19 中国石油化工股份有限公司 Crystallization and purification device and method for ethylene carbonate
CN112521363B (en) * 2019-09-19 2022-07-12 中国石油化工股份有限公司 Crystallization and purification device and method for ethylene carbonate
CN112675568A (en) * 2019-10-18 2021-04-20 中国石油化工股份有限公司 Separation and purification device and separation and purification method
CN112675568B (en) * 2019-10-18 2022-04-05 中国石油化工股份有限公司 Separation and purification device and separation and purification method
CN113893569A (en) * 2020-07-07 2022-01-07 中国石油化工股份有限公司 Static crystallization apparatus and static crystallization method
CN113893569B (en) * 2020-07-07 2023-08-04 中国石油化工股份有限公司 Static crystallization apparatus and static crystallization method
CN115177969A (en) * 2021-04-02 2022-10-14 中国石化工程建设有限公司 System and method for separating ethylbenzene from C8 aromatic hydrocarbon
CN115999316A (en) * 2021-10-21 2023-04-25 中国石油化工股份有限公司 Absorption stabilization process and absorption desorption coupling tower thereof
CN114015416A (en) * 2021-11-27 2022-02-08 浙江皇星化工股份有限公司 Production method of high latent heat energy storage material
CN114015416B (en) * 2021-11-27 2022-05-13 浙江皇星化工股份有限公司 Production method of high latent heat energy storage material

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Granted publication date: 20120530