CN106621444B - A kind of novel double down film melting crystallizer and the technique for carrying out substance separation - Google Patents
A kind of novel double down film melting crystallizer and the technique for carrying out substance separation Download PDFInfo
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- CN106621444B CN106621444B CN201611052225.7A CN201611052225A CN106621444B CN 106621444 B CN106621444 B CN 106621444B CN 201611052225 A CN201611052225 A CN 201611052225A CN 106621444 B CN106621444 B CN 106621444B
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- inner tube
- outer tube
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- falling liquid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0004—Crystallisation cooling by heat exchange
- B01D9/0013—Crystallisation cooling by heat exchange by indirect heat exchange
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0063—Control or regulation
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Abstract
The present invention relates to fusion-crystallization mode purifying substances technical fields, especially a kind of novel double down film melting crystallizer, one end of the upper housing is communicated with cold Heating medium, one end of the lower case is communicated with cold and hot matchmaker outlet, outer tube is communicated between the upper housing and lower case, and inner tube is arranged in outer tube, cold and hot matchmaker is filled between outer tube and inner tube, outer tubular tie is provided in the outer tube, and the both ends of outer tubular tie are connected in upper housing and lower case, also set is provided with outer tube falling liquid film head on the outer tube, and outer tube falling liquid film hole is offered on outer tube falling liquid film head, interior tubular tie is provided in said inner tube, and the both ends of interior tubular tie are connected in upper housing and lower case, inner tube falling liquid film head is provided in said inner tube, and inner tube falling liquid film hole is offered on inner tube falling liquid film head.The present invention guarantees that the liquid not formed a film can redistribute, and prevents the non-uniform phenomenon that forms a film caused by crystallization, guarantees film forming heat-transfer effect.
Description
Technical field
The present invention relates to fusion-crystallization mode purifying substances technical fields, more particularly to a kind of novel double falling film melt crystallizations
Device and the technique for carrying out substance separation.
Background technique
There are many multiplicity, melting crystallizer rotary drum crystallizer, surface continuous crystalizer for the form of melting crystallizer at present
(casing crystallizer), horizontal melt and dissolved crystallizer, falling-film crystallizer etc..Falling film melt crystallization device is with continuous high-efficient by more and more
Concern.
Double down film melting crystallizer has temperature control more acurrate, continuous the characteristics of being convenient for operation.
Summary of the invention
The purpose of the present invention is to solve disadvantages existing in the prior art, and the novel double down film melting of the one kind proposed
Crystallizer guarantees that the liquid not formed a film can redistribute, prevents the non-uniform phenomenon that forms a film caused by crystallization, guarantees film forming heat transfer
Effect.It is proposed a kind of accurate thermostatic control of temperature during new process realizes substance separation crystalline fusion.
To achieve the goals above, present invention employs following technical solutions:
Design a kind of novel double down film melting crystallizer, including inner tube, outer tube, upper housing and lower case, the upper housing
Top be communicated with purification material inlet and overflow bleed outlet, the bottom of the lower case is communicated with purification material outlet, described
One end of upper housing is communicated with cold Heating medium, and one end of the lower case is communicated with cold and hot matchmaker outlet, and the upper housing is under
It is communicated with outer tube between shell, and is arranged with inner tube in outer tube, cold and hot matchmaker is filled between outer tube and inner tube, is set in the outer tube
It is equipped with outer tubular tie, and the both ends of outer tubular tie are connected in upper housing and lower case, also set is provided on the outer tube
Outer tube falling liquid film head, and outer tube falling liquid film hole is offered on outer tube falling liquid film head, interior tubular tie, and interior tubular tie are provided in said inner tube
Both ends be connected in upper housing and lower case, inner tube falling liquid film head is provided in said inner tube, and open on inner tube falling liquid film head
Equipped with helical falling-film hole.
Preferably, said inner tube and inner tube tube sheet is fixed using carving type gasket, and the type gasket of carving can preferably be alleviated and set
Standby cold thermogenetic deformation adverse effect caused by equipment, guarantees the leakproofness of inner and outer tubes.
Preferably, it is provided with inner tube film forming film forming device again in said inner tube, and inner tube offers in multiple on film forming device again
Pipe overflow gas vent, be provided in the outer tube outer tube be uniformly provided with again at distributor, and on outer tube redistributor it is multiple
Outer tube overflow gas vent.
Preferably, said inner tube and outer tube are all made of poling plate sinking draining mode, arrange condensate liquid in inner and outer tubes
It is not detained.
Preferably, said inner tube falling liquid film head and outer tube falling liquid film head are all made of tangent to helix feeding structure.
The present invention also provides a kind of technique of the progress substance separation of novel double down film melting crystallizer, specifically include with
Lower step:
In use, the material for needing to purify is entered in double down film melting crystallizer by purification material inlet, is led to
The spiral inner tube falling liquid film hole crossed in inner tube falling liquid film head forms a film to material;
It is additionally provided with inner tube film forming redistributor in inner tube, redistribution film forming, inner tube film forming redistributor are carried out to separation liquid
Upper to be uniformly equipped with inner tube overflow gas vent, exhaust when for overflow and sweating after overcurrent is quick;
Material is purified after interior pipe outer wall undergoes the processes such as crystallization, sweating, melting, obtained sweat and pure liquid passes through purification
Material outlet excludes;
Hot and cold matchmaker's fluid utilizes the gasification condensation heat of solvent to make using the difference of suitable solvent boiling point at various pressures
Heat is provided to material for heating agent, provides cold energy for refrigerant using the steam raising heat heat absorption of solvent for crystallization;
Refrigerant from refrigerant inlet enter, formed a film by the helical falling-film hole in outer tube falling liquid film head to refrigerant, make it is cold
Outer wall of inner tube forms uniform film, in order to increase film-formation result, improves heat transfer efficiency, film forming redistributor pair is additionally provided in outer tube
Refrigerant carries out redistribution film forming, is uniformly equipped with overflow gas vent on outer tube film forming redistributor, guarantees that film forming is more evenly vented
Rapidly, the hot and cold matchmaker after heat exchange is exported by cold and hot matchmaker and is excluded.
Heating agent carries out sweating and melting, inner membrance redistribution to crystallized stock outside inner tube from outer tube falling liquid film head stomata and falling liquid film hole
Gas vent on device, heating steam are uniformly distributed lumen, guarantee that condensate liquid is uniform at condensation film in outer tube, overcurrent condensate liquid passes through
Overflow hole quickly flows out outer film supplying tube, guarantees to the uniform accurate constant of material heating and temperature control.
Preferably, the temperature of whole system is controlled using DCS control system, guarantees the stabilization in equipment running process
With it is efficient.
The novel double down film melting crystallizer of one kind proposed by the present invention and the technique for carrying out substance separation, beneficial effect exist
In: the novel double down film melting crystallizer arranges film forming film forming device again in inner and outer pipes, guarantees that the liquid not formed a film can be again
Distribution prevents the non-uniform phenomenon that forms a film caused by crystallization, guarantees that film forming heat-transfer effect, novel film forming distributor are provided with gas phase guiding
And liquid phase overflow hole, ensure efficiently separating for liquid phase, gas flow promotes homogeneous film formation.Double down film melting crystallizer technique mistake
Refrigerant and thermal medium in journey use suitable solvent according to different separate substance characteristics, by being saturated temperature under the full resultant pressure of difference
The temperature of the different control solvents of degree, reaches control whole system temperature stabilization and accurate, gas-liquid cycle, hot and cold alternation, crystallization
With melting process simple process, it is easy to operate, consumption it is low.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the novel double down film melting crystallizer of one kind proposed by the present invention;
Fig. 2 is the portion the A schematic enlarged-scale view of the novel double down film melting crystallizer of one kind proposed by the present invention;
Fig. 3 is the inner tube structure cross-sectional view of the novel double down film melting crystallizer of one kind proposed by the present invention;
Fig. 4 is the inner tube falling liquid film head overlooking structure diagram of the novel double down film melting crystallizer of one kind proposed by the present invention;
Fig. 5 is the inner tube film forming device plan structure signal again of the novel double down film melting crystallizer of one kind proposed by the present invention
Figure;
Inner tube and outer pipe mounting structure cross-sectional view of the Fig. 6 for the novel double down film melting crystallizer of one kind proposed by the present invention;
Fig. 7 is the outer tube falling liquid film head overlooking structure diagram of the novel double down film melting crystallizer of one kind proposed by the present invention;
Fig. 8 is that the inner tube of the novel double down film melting crystallizer of one kind proposed by the present invention and outer tube install plan structure signal
Figure;
Fig. 9 is the outer tube redistributor structural schematic diagram of the novel double down film melting crystallizer of one kind proposed by the present invention.
In figure: inner tube 1, outer tube 2, purification material inlet 3, purification material outlet 4, cold Heating medium 5, cold and hot matchmaker outlet 6,
Inner tube falling liquid film head 7, outer tube falling liquid film head 8, overflow bleed outlet 9, inner tube again film forming device 10, carve type gasket 11, interior tubular tie 12, inner tube
Falling liquid film hole 13, inner tube overflow gas vent 14, outer tubular tie 15, outer tube redistributor 16, outer tube falling liquid film hole 17, outer tube overflow exhaust
Hole 18, upper housing 19, lower case 20.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.
Referring to Fig.1-9, a kind of novel double down film melting crystallizer, including inner tube 1, outer tube 2, upper housing 19 and lower case
20, the top of upper housing 19 is communicated with purification material inlet 3 and overflow bleed outlet 9, and the bottom of lower case 20 is communicated with purification
Material outlet 4, one end of upper housing 19 are communicated with cold Heating medium 5, and one end of lower case 20 is communicated with cold and hot matchmaker outlet 6, upper casing
It is communicated with outer tube 2 between body 19 and lower case 20, and is arranged with inner tube 1 in outer tube 2, fixed plate is additionally provided on the outside of inner tube 1, it is interior
Type gasket 11 is carved between pipe 1 and the fixed plate of inner tube 1, and carve type gasket 11 can preferably alleviate the cold thermogenetic deformation of equipment
The adverse effect caused by equipment guarantees the leakproofness of inner tube 1 and outer tube 2, is provided with inner tube film forming device 10 again in inner tube 1, and
Inner tube offers multiple inner tube overflow gas vents 14 on film forming device 10 again, is provided with outer tube redistributor 16, and outer tube in outer tube 2
It is uniformly provided with multiple outer tube overflow gas vents 18 on redistributor 16, guarantees what feed liquid on inner tube redistributor 10 was not easy to crystallize
Make film forming simultaneously more evenly.
Cold and hot matchmaker is filled between outer tube 2 and inner tube 1, inner tube 1 and outer tube 2 are all made of poling plate sinking draining mode, arrange
Condensate liquid is not detained in inner tube 1 and outer tube 2.
Outer tubular tie 15 is provided in outer tube 2, and the both ends of outer tubular tie 15 are connected to upper housing 19 and lower case
On 20, also set is provided with outer tube falling liquid film head 8 on outer tube 2, and outer tube falling liquid film hole 17 is offered on outer tube falling liquid film head 8, sets in inner tube 1
It is equipped with interior tubular tie 12, and the both ends of interior tubular tie 12 are connected in upper housing 19 and lower case 20, are provided in inner tube 1
Inner tube falling liquid film head 7, and inner tube falling liquid film hole 13 is offered on inner tube falling liquid film head 7, inner tube falling liquid film head 7 is all made of with outer tube falling liquid film head 8
Tangent to helix feeding structure.
The present invention also provides a kind of technique of the progress substance separation of novel double down film melting crystallizer, specifically include with
Lower step:
In use, the material for needing to purify is entered in double down film melting crystallizer by purification material inlet 4, is led to
The spiral inner tube falling liquid film hole 13 crossed in inner tube falling liquid film head 7 forms a film to material;
It is additionally provided with inner tube redistributor 10 in inner tube 1, redistribution film forming is carried out to melt liquid, at inner tube redistributor 10
It is upper to be uniformly equipped with inner tube overflow gas vent 14;
After 1 outer wall of pipe successively undergoes the processes such as crystallization, sweating, melting including purification material, obtained sweat and pure liquid is logical
Cross the exclusion of purification material outlet 4;
Hot and cold matchmaker's fluid utilizes the gasification condensation heat of solvent to make using the difference of suitable solvent boiling point at various pressures
Heat is provided to material for heating agent, provides cold energy for refrigerant using the steam raising heat heat absorption of solvent for crystallization;
Cold and hot matchmaker enters from cold Heating medium 5, by the spiral inner tube falling liquid film hole 17 in outer tube falling liquid film head 8 to cold and hot matchmaker into
Row film forming, makes hot and cold matchmaker form uniform film in 1 outer wall of inner tube, in order to increase film-formation result, improves heat transfer efficiency, in outer tube 2
It is additionally provided with inner tube redistributor 16 and redistribution film forming is carried out to cold and hot matchmaker, at uniformly excessive equipped with inner tube on outer tube redistributor 16
Gas vent 18 is flowed, guarantees to make film forming while feed liquid is not easy to crystallize on redistributor 18 more evenly, the hot and cold matchmaker after heat exchange passes through
Cold and hot matchmaker outlet 6 excludes.
The temperature of whole system is controlled using DCS control system, guarantees stabilization in equipment running process and efficiently.
More than, it is merely preferred embodiments of the present invention, but scope of protection of the present invention is not limited thereto, it is any
Those familiar with the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its invents
Design is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (6)
1. a kind of double down film melting crystallizer, including inner tube (1), outer tube (2), upper housing (19) and lower case (20), it is described on
The top of shell (19) is communicated with purification material inlet (3) and overflow bleed outlet (9), and the bottom of the lower case (20) is communicated with
It purifies material outlet (4), it is characterised in that: one end of the upper housing (19) is communicated with cold Heating medium (5), the lower case
(20) one end is communicated with cold and hot matchmaker and exports (6), is communicated with outer tube (2) between the upper housing (19) and lower case (20), and
It is arranged with inner tube (1) in outer tube (2), cold and hot matchmaker is filled between outer tube (2) and inner tube (1), be provided in the outer tube (2) outer
Tubular tie (15), and the both ends of outer tubular tie (15) are connected on upper housing (19) and lower case (20), the outer tube (2)
On also set be provided with outer tube falling liquid film head (8), and outer tube falling liquid film hole (17) is offered on outer tube falling liquid film head (8), in said inner tube (1)
It is provided with interior tubular tie (12), and the both ends of interior tubular tie (12) are connected on upper housing (19) and lower case (20), institute
It states and is provided with inner tube falling liquid film head (7) on inner tube (1), and offer inner tube falling liquid film hole (13), said inner tube on inner tube falling liquid film head (7)
(1) inner tube film forming device (10) again are provided in, and inner tube offers multiple inner tube overflow gas vents (14) on film forming device (10) again,
It is provided with outer tube film forming device (16) again in the outer tube (2), and outer tube is uniformly provided with multiple outer tubes on film forming device (16) again and overflows
It flows gas vent (18).
2. a kind of double down film melting crystallizer according to claim 1, which is characterized in that also set on the outside of said inner tube (1)
It is equipped with fixed tube sheet, type gasket (11) are carved between said inner tube (1) and the fixed tube sheet of inner tube (1), and carves type gasket (11)
The cold thermogenetic deformation adverse effect caused by equipment of equipment can preferably be alleviated, guarantee the sealing of inner tube (1) and outer tube (2)
Property.
3. a kind of double down film melting crystallizer according to claim 1, which is characterized in that the outer tube (2) uses poling
Plate sinking draining mode, condensate liquid are not detained in equipment.
4. a kind of double down film melting crystallizer according to claim 1, which is characterized in that said inner tube falling liquid film head (7) with
Outer tube falling liquid film head (8) is all made of tangent to helix feeding structure.
5. the technique that a kind of double down film melting crystallizer according to claim 1 carries out substance separation, it is characterised in that: tool
Body the following steps are included:
In use, the material for needing to purify is entered in double down film melting crystallizer by purification material inlet (4), is passed through
Spiral inner tube falling liquid film hole (13) in inner tube falling liquid film head (7) form a film at inner tubal wall to material;
Inner tube is additionally provided in inner tube (1), and film forming device (10) carries out redistribution film forming, inner tube redistributor (10) to melt liquid again
It is upper to be uniformly equipped with inner tube overflow gas vent (14);
After purification material manages the processes such as the crystallization of (1) outer wall experience, sweating, melting inside, obtained sweat and pure liquid passes through purification
Material outlet (4) excludes;
Hot and cold matchmaker's fluid using suitable solvent boiling point at various pressures difference, using the gasification condensation heat of solvent as hot
Matchmaker provides heat to material, provides cold energy for refrigerant using the steam raising heat heat absorption of solvent for crystallization;
Refrigerant from refrigerant inlet (5) enter, by falling liquid film hole (17) in the spiral in outer tube falling liquid film head (8) to refrigerant carry out at
Film, make it is cold form uniform film in inner tube (1) outer wall, in order to increase film-formation result, improve heat transfer efficiency, outer tube is also set in (2)
There is outer tube to carry out redistribution film forming to refrigerant at distributor (16) again, is uniformly equipped with overflow in film forming redistributor (16) and arranges
Stomata (18), guarantees outer wall of inner tube refrigerant film forming more evenly inner tube crystallization temperature constant temperature, and the hot and cold matchmaker after heat exchange passes through cold and hot matchmaker
(6) are exported to exclude.
6. the technique that a kind of double down film melting crystallizer according to claim 5 carries out substance separation, which is characterized in that whole
The temperature of a system is controlled using DCS control system, guarantees stabilization in equipment running process and efficiently.
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CN201611052225.7A CN106621444B (en) | 2016-11-25 | 2016-11-25 | A kind of novel double down film melting crystallizer and the technique for carrying out substance separation |
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CN106621444B true CN106621444B (en) | 2019-08-23 |
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CN109045743A (en) * | 2018-08-29 | 2018-12-21 | 江苏德邦工程有限公司 | The novel double down film melting crystallizer of one kind and its substance separating technology |
CN114405050B (en) * | 2022-01-14 | 2024-08-27 | 上海东庚化工技术有限公司 | Continuous rotational flow falling film melting crystallizer |
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US4552575A (en) * | 1982-02-04 | 1985-11-12 | Ruetgerswerke Aktiengesellschaft | Method for the mass separation of a liquid mixture through fractional crystallization |
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Family Cites Families (1)
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CN102282120B (en) * | 2009-02-03 | 2015-03-04 | 株式会社日本触媒 | Process for production of (meth)acrylic acid |
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2016
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US4552575A (en) * | 1982-02-04 | 1985-11-12 | Ruetgerswerke Aktiengesellschaft | Method for the mass separation of a liquid mixture through fractional crystallization |
CN202128924U (en) * | 2011-06-20 | 2012-02-01 | 李锦龙 | Falling film evaporator for sandwich layer pipelines |
CN202802799U (en) * | 2012-05-11 | 2013-03-20 | 合肥宁垣工程技术有限责任公司 | Film falling liquid distributor |
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 |
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