CN109692496A - Strengthen the method for fluidisation heat transfer crystallization - Google Patents
Strengthen the method for fluidisation heat transfer crystallization Download PDFInfo
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- CN109692496A CN109692496A CN201710982588.9A CN201710982588A CN109692496A CN 109692496 A CN109692496 A CN 109692496A CN 201710982588 A CN201710982588 A CN 201710982588A CN 109692496 A CN109692496 A CN 109692496A
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- crystallizer
- tube side
- heat transfer
- heat exchanger
- fluidisation
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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
- B01D9/0059—General arrangements of crystallisation plant, e.g. flow sheets
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D2009/0086—Processes or apparatus therefor
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- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of methods for strengthening fluidisation heat transfer crystallization, are suitable for the online block clearing of petrochemical industry heat exchanger, are also applied for the cooling technique for reaching saturation and crystallizing of solution, are particularly suitable for the crystallization processes such as paraxylene, glycolide.The present invention uses spiral-flow type feeding manner, and unique root canal journey is arranged, and the upper end of tube side is equipped with solid-liquor separation room, particle outlet and taphole, and lower end is equipped with solid particle blanking device and tube side tangential inlet.Reinforcing fluidisation heat transfer method for crystallising of the invention has the characteristics that solid holdup is low, scouring force is strong, scale removal is high-efficient.
Description
Technical field
The invention belongs to petrochemical industry, in particular to a kind of reinforcing fluidisation heat transfer method for crystallising.
Technical background
Double-pipe chiller is commonly used in crystallization processes, it is will to complete in the inner tube of material solution input double-pipe chiller.
The technique includes crystal system, separation system and refrigeration system.Material solution is inputted into crystal system, in the set that several levels are concatenated into
Pipe crystallizer inner tube flow forward, the cryogen through outer tube take heat, material solution are made gradually to cool down, and form crystal grain, and scraper will
The crystal tied in inner tubal wall scrapes in time, until material solution reaches filtration temperature, feeding separation system.Separation system centrifugation
Machine isolates crystal and mother liquor；It is effective to make cryogen, what rear set for what casing oil liquid (cold filtrate) before refrigeration system usually makes
Cryogen exchanges heat with material solution.There are many disadvantages for double-pipe chiller crystallization processes, and such as there is wrap in serious crystal
Phenomena such as impure, thus lead to that product yield is low, purity is low, overall heat-transfer coefficient is low, equipment is expensive and need to often repair, repair
It is costly, power consumption is big etc..
Patent US3642195 and US3681230 disclose a kind of technique that part tubular crystallizer is replaced with scrubbing tower, claim
Wash tower process.Enter scrubbing tower after raw material is pre-cooled, tower is divided into several segments, and every section has stirring, while low through nozzle spray people
Warm solvent.Every section is gathered cold phenomenon by injection mixing and stirring action elimination, is inhibited the generation of new nucleus, is enable crystal preferably
It grows up.Since to every section of temperature drop strict control, gained crystal is larger.Therefore, in filtering velocity, product yield, product purity and energy consumption
Aspect all makes moderate progress.But the technique is there are still some shortcomings, as could more after scrubbing tower is huge, nozzle easily blocks shut-down
The temperature for changing, going out cooling tower, which can only achieve 0 DEG C or so, also needs a certain number of double-pipe chillers as rear cold, thus its application
It is restricted, industrialized unit is few.
D.G.Klaren in 1989 etc. proposes that one kind is followed in the U.S. " Hydrocarbon processing " 68 (7) P48-50
The fluidized-bed crystallizer of ring type replaces double-pipe chiller.For the crystallizer such as vertical shell-and-tube heat exchanger, composition includes many
Item is parallel to each other and upright tube side and several circulation pipes, solid particulate distributions plate and the tubular with upper chamber and lower room
Shell.Solid particle is mixed and is fluidized in lower room with the solution for entering crystallizer, is entered in each tube side through distribution grid, and flowing
Enter upper chamber under change state.Since upper chamber sectional area is big compared with tube side, flow velocity decline, liquid is separated admittedly.Solution is together with crystal
By flowing out crystallizer through outlet at the top of upper chamber, and solid particle then settles down and returns to lower room through circulation pipe, then crystallizes with entering
The solution of device mixes, it is intended to realize that the liquid that solid particle constantly recycles consolidates fluid mapper process.In tube side, if fluidization solid particle
Constantly tube wall is washed away, the boundary layer of tube wall can be not only destroyed, but also crystal on tube wall can be removed, heat transfer coefficient can be made significantly to mention
It is high.
Chinese patent CN99117748.7, CN200920196356.1, CN201620923885.7, CN1995890N, CN
102759289 A, CN 103629837 A also successively disclose fluid-bed heat exchanger and attached inner member, such as be separated by solid-liquid separation
CN200610134381.8 etc..
But at present it is this it is circulating fluid bed be not successfully applied to crystallization process, reason is this circulation
Formula fluidized bed is the solid particle for distributing each tube side by distribution grid, and substantially its snaking acts on very little, not can guarantee fluidisation
Solid particle is uniformly distributed in numerous tube sides, therefore the fluidized state of each tube side is different, also different to tube wall scouring capability.Punching
The weak tube side crystal of brushing force is thick, and resistance is bigger, further decreases flow, and it is stifled that this vicious circle eventually leads to part tube side
Plug, it is ineffective.In addition, circulation pipe flow velocity is excessively slow, the flowing of stratum granulosum is difficult to wash away by crystal, is crystallized object quickly
It blocks, destroys the circulation of solid particle, carry out crystallization process can not.
The present invention is directed to overcome, the particle of the prior art is low with tube wall effective collision frequency, defect of scale removal effect difference.
Summary of the invention
, punching low with tube wall effective collision frequency that the technical problem to be solved by the present invention is to particles existing in the prior art
Brushing force is weak, scale removal effect difference problem；A kind of method for strengthening fluidisation heat transfer crystallization is provided, this method utilizes fluid-bed heat exchanger
The mode of tube-side inlet tangential admission has the characteristics that solid holdup is low, scouring force is strong, scale removal is high-efficient.
In order to solve the above technical problems, the present invention is as follows using technical solution:
A method of reinforcing fluidisation heat transfer crystallization, using fluidisation heat transfer crystallizer, the fluidisation heat transfer crystallizer includes
Shell side, tube side, particle blanking device, equipment for separating liquid from solid and circulating water chennel, it is characterised in that set in fluidized bed heat exchanger crystallizer
There is a unique tube side, tube side is provided with solid particle, and raw material tangentially enters along tube-side inlet, and spiral-flow type is formed in tube side
Upper up-flow.
In above-mentioned technical proposal, it is preferable that eddy flow charging is realized through tangential feed or in the way of deflector.
In above-mentioned technical proposal, it is preferable that the quantity of fluidized bed heat exchanger crystallizer total pipe range according to needed for total temperature drop and stream
Depending on heat exchange area needed for changing bed heat exchange crystallizer, the tube side internal diameter diameter of fluidized bed heat exchanger crystallizer is 20 millimeters -500 millimeters
Seamless steel pipe, heat exchanger cooling section height is at 2 meters -20 meters.More preferably, the tube side internal diameter diameter of fluidized bed heat exchanger crystallizer
For 20 millimeters of -100 millimeters of seamless steel pipes, heat exchanger cooling section height is at 5 meters -10 meters.
In above-mentioned technical proposal, it is preferable that the operation temperature of fluidized bed heat exchanger crystallizer: tube side is -55 DEG C~70 DEG C；Shell
Journey is -55 DEG C~110 DEG C.
In above-mentioned technical proposal, it is preferable that setting fluidized bed heat exchanger crystallizer bed height measuring instrument detects consolidating for prepackage
Body particle.
In above-mentioned technical proposal, it is preferable that cryogen used in fluidized bed heat exchanger crystallizer shell side is water, freon, ammonia, third
Alkane or filtrate.According to different cryogens, optimization design shell side diameter, heat exchanger structure and reinforcing means etc. are optimal to guarantee
Overall heat-transfer coefficient makes the economical rationality of industrialized unit.
In above-mentioned technical proposal, it is preferable that at least one taphole is arranged in fluidized-bed crystallizer tube side top.
In above-mentioned technical proposal, it is preferable that the density of solid particle is higher than the density of raw material.More preferably, solid
Grain is porcelain ball, steel wire or aluminum oxide particle.
In above-mentioned technical proposal, it is preferable that the ratio of the equivalent diameter of solid particle and tube side caliber is 1/5-1/15.
In above-mentioned technical proposal, it is preferable that the heat transfer of shell side cryogen can be used thermal siphon and rise membrane technology or falling liquid film technology.Hot rainbow
The liquid phase cryogen gravity flow of suction membrane technology, that is, flash-pot outflow from heat exchanger shell pass bottom enter with after oil liquid heat exchange, part
Vapour-liquid mixed phase is recycled back into evaporator and carries out vapor-liquid separation after vaporization；Falling liquid film technology is i.e. to each section of addition cryogen of heat exchanger, accordingly
Enter concetrated pipe Returning evaporimeter after each section of heat exchanger vaporization and carries out vapor-liquid separation.
In above-mentioned technical proposal, it is preferable that adoptable in order to improve the heat transfer coefficient of fluidized bed heat exchanger crystallizer shell side
Augmentation of heat transfer means are such as: processing surface, rough surface, extended surface, eddy-currents, porous structure, helix tube, slotted-tube, induction
250-2000w/m of the structures such as stream, finned tube, porous surface to further increase2DEG C overall heat-transfer coefficient.
The present invention also provides a kind of reinforcings to fluidize heat transfer crystallizer, including shell side, tube side, particle blanking device, solid-liquid point
From device and circulating water chennel, a unique tube side is equipped in fluidized bed heat exchanger crystallizer, tube side is provided with solid particle, raw material edge
Tube-side inlet tangentially enter, spiral-flow type upper up-flow is formed in tube side, the rear portion of tube side is equipped with liquid-solid separation device, and particle follows
Particle blanking device is provided in loop back path.
In above-mentioned technical proposal, it is preferable that eddy flow charging is realized through tangential feed or in the way of deflector.
In above-mentioned technical proposal, it is preferable that the quantity of fluidized bed heat exchanger crystallizer total pipe range according to needed for total temperature drop and stream
Depending on heat exchange area needed for changing bed heat exchange crystallizer, the tube side internal diameter diameter of fluidized bed heat exchanger crystallizer is 20 millimeters -500 millimeters
Seamless steel pipe, heat exchanger cooling section height is at 2 meters -20 meters.More preferably, the tube side internal diameter diameter of fluidized bed heat exchanger crystallizer
For 20 millimeters of -100 millimeters of seamless steel pipes, heat exchanger cooling section height is at 5 meters -10 meters.
In above-mentioned technical proposal, it is preferable that the operation temperature of fluidized bed heat exchanger crystallizer: tube side is -55 DEG C~70 DEG C；Shell
Journey is -55 DEG C~110 DEG C.
In above-mentioned technical proposal, it is preferable that setting fluidized bed heat exchanger crystallizer bed height measuring instrument detects consolidating for prepackage
Body particle.
In above-mentioned technical proposal, it is preferable that cryogen used in fluidized bed heat exchanger crystallizer shell side is water, freon, ammonia, third
Alkane or filtrate.According to different cryogens, optimization design shell side diameter, heat exchanger structure and reinforcing means etc. are optimal to guarantee
Overall heat-transfer coefficient makes the economical rationality of industrialized unit.
In above-mentioned technical proposal, it is preferable that at least one taphole is arranged in fluidized-bed crystallizer tube side top.
In above-mentioned technical proposal, it is preferable that the density of solid particle is higher than the density of raw material.More preferably, solid
Grain is porcelain ball, steel wire or aluminum oxide particle.
In above-mentioned technical proposal, it is preferable that the ratio of the equivalent diameter of solid particle and tube side caliber is 1/5-1/15.
In above-mentioned technical proposal, it is preferable that the heat transfer of shell side cryogen can be used thermal siphon and rise membrane technology or falling liquid film technology.Hot rainbow
The liquid phase cryogen gravity flow of suction membrane technology, that is, flash-pot outflow from heat exchanger shell pass bottom enter with after oil liquid heat exchange, part
Vapour-liquid mixed phase is recycled back into evaporator and carries out vapor-liquid separation after vaporization；Falling liquid film technology is i.e. to each section of addition cryogen of heat exchanger, accordingly
Enter concetrated pipe Returning evaporimeter after each section of heat exchanger vaporization and carries out vapor-liquid separation.
In above-mentioned technical proposal, it is preferable that adoptable in order to improve the heat transfer coefficient of fluidized bed heat exchanger crystallizer shell side
Augmentation of heat transfer means are such as: processing surface, rough surface, extended surface, eddy-currents, porous structure, helix tube, slotted-tube, induction
250-2000w/m of the structures such as stream, finned tube, porous surface to further increase2DEG C overall heat-transfer coefficient.
The present invention uses fluidized bed heat exchanger crystallizer, is fed using spiral-flow type, each parameter in regulation heat exchange crystallizer, fluidisation
The overall heat-transfer coefficient of bed heat exchange crystallizer is 4-5 times of double-pipe chiller, can greatly reduce heat transfer area and operating cost；Solution
Heat transfer efficiency of having determined is low, the problem that distribution of particles effect is poor, product purity and yield are low, in particular with spiral-flow type entrance, produces
The function and effect of raw eddy flow field, so that solid particle scrapes tube wall under the influence of centrifugal force, in identical solid holdup, apparently
Under flow velocity, function and effect (or scaling effect) are the 2 times or more of existing fluidized bed heat exchanger crystallizer, and product yield is made to compare casing
Crystallizer technique improves 2%-5%；Equipment is simple, investment is low, maintenance cost is extremely low；Simple process does not have to electric scraper, thus
Energy consumption is also low.
The present invention is the rising crystallizer of crystallization processes.
Detailed description of the invention
Fig. 1 is spiral-flow type single tube external circulation fluidized bed multitube heat transfer crystallizer of the present invention.
In figure, 1- shell side, 2- tube side, 3- liquid-solid separator, 4- solid particle blanking device, 5- centrifugal pump, 6- recirculated water
Slot Fig. 2 is crystallizer spiral-flow type feeding inlet structural schematic diagram.
Specific embodiment
Below by embodiment, the present invention is further elaborated.
[embodiment 1]
The crystallization process of paraxylene in mixed xylenes, spiral-flow type single tube external circulation fluidized bed multitube as described in Figure 1
It exchanging heat in crystallizer, mixed xylenes raw material is entered the bottom of fluidized bed heat exchanger crystallizer by 2 feed inlet tangential inlet of tube side, by
Enter in tangent line, material is made to form the eddy flow of rising in tube side 2, this type of flow not only increases solid particle and tube wall
Frictional strength and frequency are also beneficial to particle being uniformly distributed in pipeline.Liquid nitrogen is by 1 upper end of fluidized bed heat exchanger crystallizer shell side
Cryogen entrance enter in shell side, in tube side material carry out counterflow heat exchange.Cryogen after heat exchange is crystallized by fluidized bed heat exchanger
The cryogen of 1 lower part of device shell side exports discharge, after material completes heat exchange by fluidized bed heat exchanger crystallizer tube side 2, by solid-liquid point
From device 3.It is separated in 3 endoparticle of equipment for separating liquid from solid, is discharged from the underflow opening of liquid-solid separator, and material is consolidated by liquid
The top exit of separator is discharged, and is squeezed into fluidized bed heat exchanger crystallizer again through centrifugal pump 5.From 3 underflow opening of liquid-solid separator
The solid particle of discharge is further enriched with through down-comer, in the realization blanking of solid particle blanking device 4 of decline bottom of the tube, and by
Liquid is brought into fluidized bed heat exchanger crystallizer, and a circulation is completed.
The tube side internal diameter of fluidized bed heat exchanger crystallizer be 300 mm diameter seamless steel pipe, 2 meters of cooling section height, tube side -15
DEG C, -20 DEG C of shell side, solid particle is porcelain ball, and the ratio of equivalent diameter and 2 caliber of tube side is 1/6, solid holdup 2%.
Through 72 hours continuous operations, spiral-flow type single tube external circulation fluidized bed multitube heat transfer crystallizer did not occurred tying wall phenomenon,
Overall heat-transfer coefficient is stably maintained at 1620w/m2DEG C, and the paraxylene crystals that average particle size is 200 μm can be obtained.
[embodiment 2]
Process flow is identical with [embodiment 1], and the tube side internal diameter of fluidized bed heat exchanger crystallizer is 30 millimeters of seamless steels of diameter
Pipe, 20 meters of cooling section height, -15 DEG C of tube side, -55 DEG C of shell side, solid particle is porcelain ball, equivalent diameter and 2 caliber of tube side
Ratio is 1/6, solid holdup 5%.Through 72 hours continuous operations, spiral-flow type single tube external circulation fluidized bed multitube conducted heat crystallizer not
There is knot wall phenomenon, overall heat-transfer coefficient is stably maintained at 1750w/m2DEG C, and the paraxylene that average particle size is 350 μm can be obtained
Crystal.
[comparative example 1]
Using double-pipe chiller, tube side internal diameter is 80 millimeters of seamless steel pipes of diameter, 2 meters of cooling section height, -15 DEG C of tube side,
- 20 DEG C of shell side, occur knot wall phenomenon through 72 hours continuous operations, in double-pipe chiller, overall heat-transfer coefficient be stably maintained at by
1500w/m2DEG C it is gradually decreased to 520w/m2DEG C, obtain the paraxylene crystals that average particle size is 120 μm.
[comparative example 2]
Process flow is identical with [embodiment 1], but entrance does not use spiral-flow type entrance, the pipe of fluidized bed heat exchanger crystallizer
Journey internal diameter is 30 millimeters of seamless steel pipes of diameter, and 20 meters of cooling section height, -15 DEG C of tube side, -55 DEG C of shell side, solid particle is porcelain ball,
The ratio of its equivalent diameter and 2 caliber of tube side is 1/6, solid holdup 5%.Overall heat-transfer coefficient is stably maintained at by 1500w/m2℃
It is gradually decreased to 1000w/m2℃。
Obviously, using method of the invention, there is biggish technical advantage, in the industrial production that can be used for crystallizing.
Claims (10)
1. a kind of method for strengthening fluidisation heat transfer crystallization, using the crystallizer that conducts heat is fluidized, the fluidisation heat transfer crystallizer includes shell
Journey, tube side, particle blanking device, equipment for separating liquid from solid and circulating water chennel, it is characterised in that be equipped in fluidized bed heat exchanger crystallizer
A unique tube side, tube side are provided with solid particle, and raw material tangentially enters along tube-side inlet, are formed in spiral-flow type in tube side
Up-flow.
2. it is according to claim 1 strengthen fluidisation heat transfer crystallization method, which is characterized in that eddy flow charging by tangent line into
Material is realized in the way of deflector.
3. the method according to claim 1 for strengthening fluidisation heat transfer crystallization, it is characterised in that fluidized bed heat exchanger crystallizer
Quantity depending on heat exchange area needed for total pipe range needed for total temperature drop and fluidized bed heat exchanger crystallizer, fluidized bed heat exchanger crystallizer
Tube side internal diameter diameter is 20 millimeters of -500 millimeters of seamless steel pipes, and heat exchanger cooling section height is at 2 meters -20 meters.
4. the method according to claim 1 for strengthening fluidisation heat transfer crystallization, it is characterised in that fluidized bed heat exchanger crystallizer
Operation temperature: tube side is -55 DEG C~70 DEG C；Shell side is -55 DEG C~110 DEG C.
5. the method according to claim 1 for strengthening fluidisation heat transfer crystallization, it is characterised in that setting fluidized bed heat exchanger crystallizes
Device bed height measuring instrument, detects the solid particle of prepackage.
6. the method according to claim 1 for strengthening fluidisation heat transfer crystallization, which is characterized in that fluidized bed heat exchanger crystallizer shell
The cryogen of Cheng Suoyong is water, freon, ammonia, propane or filtrate.
7. the method according to claim 1 for strengthening fluidisation heat transfer crystallization, it is characterised in that on fluidized-bed crystallizer tube side
At least one taphole is arranged in portion.
8. the method according to claim 1 for strengthening fluidisation heat transfer crystallization, it is characterised in that the density of solid particle is higher than
The density of raw material.
9. the method according to claim 1 for strengthening fluidisation heat transfer crystallization, it is characterised in that the equivalent diameter of solid particle
Ratio with tube side caliber is 1/5-1/15.
10. a kind of reinforcing fluidisation heat transfer crystallizer, which is characterized in that including shell side, tube side, particle blanking device, be separated by solid-liquid separation
Device and circulating water chennel, are equipped with a unique tube side in fluidized bed heat exchanger crystallizer, and tube side is provided with solid particle, raw material along
Tube-side inlet tangentially enters, and spiral-flow type upper up-flow is formed in tube side, and the rear portion of tube side is equipped with liquid-solid separation device, particle circulation
Particle blanking device is provided on circuit.
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| CN201710982588.9A CN109692496A (en) | 2017-10-20 | 2017-10-20 | Strengthen the method for fluidisation heat transfer crystallization |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113074565A (en) * | 2021-04-06 | 2021-07-06 | 南京炼油厂有限责任公司 | Liquid-phase rotational flow mixing liquid-reducing automatic impurity-removing heat exchanger and process method and application thereof |
| CN113819776A (en) * | 2021-08-11 | 2021-12-21 | 自然资源部天津海水淡化与综合利用研究所 | Cyclone fluidized bed |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113074565A (en) * | 2021-04-06 | 2021-07-06 | 南京炼油厂有限责任公司 | Liquid-phase rotational flow mixing liquid-reducing automatic impurity-removing heat exchanger and process method and application thereof |
| CN113819776A (en) * | 2021-08-11 | 2021-12-21 | 自然资源部天津海水淡化与综合利用研究所 | Cyclone fluidized bed |
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Application publication date: 20190430 |