CN106166400B - A kind of dilution crystallization device and method of film auxiliary control - Google Patents
A kind of dilution crystallization device and method of film auxiliary control Download PDFInfo
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- CN106166400B CN106166400B CN201610639463.1A CN201610639463A CN106166400B CN 106166400 B CN106166400 B CN 106166400B CN 201610639463 A CN201610639463 A CN 201610639463A CN 106166400 B CN106166400 B CN 106166400B
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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
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/005—Selection of auxiliary, e.g. for control of crystallisation nuclei, of crystal growth, of adherence to walls; Arrangements for introduction thereof
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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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- 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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Abstract
The present invention provides the dilution crystallization technique device and method of a kind of auxiliary control of film, belong to crystallization field of engineering technology.Solution to be crystallized is added in head tank, and dissolved agent is added in material liquid tank, is opened electronic balance, computer, stirring and temperature regulating device, after system is stablized, is opened the peristaltic pump of material liquid tank, dissolved agent is circulated between material liquid tank and membrane module；After dissolved agent stable circulation, opening the peristaltic pump being connected with head tank makes crystallization solution be passed through membrane module.The dissolved agent come into full contact with membrane module and crystallization solution can flow into external storage tank in membrane module and be filtered and post-processed after nucleating growth；Also can outside membrane module nucleating growth, after solute all separate out after filter.Electronic balance records the addition of dissolved agent in real time, systematically regulates and controls the addition of dissolved agent by the control to film and operating condition, and then obtain preferable crystal product.
Description
Technical field
The invention belongs to crystallize field of engineering technology, particularly suitable for the preparation of some crystals and to crystalline product
There is the production process of strict demand, broader space is provided for the development of dilution crystallization technology.
Background technology
Dilution crystallization is a kind of common separation method, it is by adding dissolved agent into solution so that solute is in original
Solubility in solvent declines, so as to produce degree of supersaturation, makes solute that the process for crystallizing and being separated out from solution occur.Add
Dissolved agent can be gas or liquid.For dilution crystallization compared to other crystallization process, system does not have the change of temperature, can be significantly
The yield of crystal product is improved, is played the role of in crystallization art important.In recent years, being widely applied to of dilution crystallization
The every field such as work, food, pharmacy.Social development and the continuous lifting of industrial requirement cause the requirement for crystalline product also to be got over
Come higher, especially pharmaceutical industry has more and more particular/special requirements for the pattern of crystal, size distribution, particle diameter etc..Therefore, no
Further investigate disconnectedly and optimize dilution crystallization process and have great importance.
During dilution crystallization, dissolved agent, which is added dropwise, can cause the degree of supersaturation of addition point higher, will produce moment largely
Nucleus and reunite, the nucleus produced under the conditions of this tends to contain mother liquor, and then influences the quality of crystalline product.At present
Industrial process in, mainly have following two dissolved agent feed postitions：(1) stirring-type is added dropwise, this mode is to utilize dropper etc.
Dissolved agent is added dropwise into external crystallizer for instrument, while is thoroughly mixed with blender.This method is the simplest, application
At most, but its shortcoming is also apparent from：Such a method adds dissolved agent it is difficult to ensure that the degree of supersaturation of solution is uniform in crystallizer
Distribution, the limited diffusion rates of dissolved agent drop, the supersaturated horizontal ratio being added dropwise a little is much higher elsewhere, therefore this side
Formula will cause outburst to be nucleated, while produce a large amount of primary nucleus for containing mother liquor, cause product size uneven, size distribution
Wide, product quality declines；(2) external mix feed type, this mode are to improve the admixture of dissolved agent and solution
And a kind of novel jet-type feed arrangement developed, it is divided into two kinds, one kind is to be directly injected into material pattern, and another kind is outer follows
Ring sprayed feed pattern.Both of which mainly improves to a certain extent mixes non-uniform defect, but the crystalline substance formed
Bulk structural defect is more；Turbulence intensity compares Gao Shihui and causes that crystal nucleation is more and growth rate is small.
In Chinese patent CN021152070.4,200610165255.9,201210594123.3 and 201310694016.2
Refer to prepare medicine and biological macromolecule crystal with dilution crystallization can obtain satisfactory crystal product.But patent
In the dilution crystallization mentioned all be the production process that stirring-type is added dropwise, it is poor to the controlling of operating condition, production extension compared with
Difficulty, the species for producing crystal also have limitation very much.And the optimization carried out in patent to dilution crystallization, is more molten in crystallization
Improved in the pre-treatment of liquid, for dilution crystallization, this main production link does not improve, thus crystal product matter
The raising of amount is very limited, it is also difficult to which different dilution crystallization systems are promoted the use of.
In pharmacy and chemical industry, some new coupling process and mixing apparatus can improve dissolved knot to a certain extent
The defects of brilliant, but cannot still solve the problems, such as that degree of supersaturation skewness, outburst nucleation and crystal are reunited.Therefore, only
It is far from being enough to be confined to pre-treatment and the improvement of hybrid mode, it should more to be directed to dilution crystallization technology in itself
Research, changes traditional dissolved agent feed postition, inherently the defects of removal dilution crystallization.
UF membrane is a kind of efficient, energy-saving and environmental protection, simple process technology, has nowadays been applied in every field
Quite extensively, researcher have developed diversified membrane separating process for different industrial requirements.Meanwhile membrane separation technique
With other technologies coupling integration, the advantage of membrane separating process can be given full play to so that industrial process is strengthened, process efficiency
All get a promotion with controlling extent.
With the continuous development of membrane material science, and the further investigation to UF membrane and dilution crystallization technology, some property
The relatively good film of energy can be used in various membrane separating process.The organic and inorganic membrane material that can be prepared now has good
Hydrophobicity, corrosion resistance and mechanical performance.Meanwhile the membrane material of various forms causes the filling rate of membrane module to greatly promote,
Assembly volume greatly reduces, and installation cost further reduces, and is easy to integrate with other devices.With membrane separation technique increasingly into
Ripe, pressure differential, temperature difference, concentration difference by regulating and controlling film both sides etc., realize transmembranal penetration and the transmission of liquid.It is of the invention abundant
The advantage of membrane material and membrane separation technique is applied, changes the feed postition of dissolved agent, traditional dropwise addition stirring-type is changed into
Film adds formula, dissolved agent and crystallization solution is contacted mixing in membrane module, reaches hypersaturated state.Solute can be in membrane module
Crystallization, can also discharge membrane module and be crystallized in exterior crystallizer, mainly be modified by the control to operating condition and the selection of film
Obtain preferable crystal product.The invention is mainly used for the preparation of medicine and chemical products, has widened answering for dilution crystallization significantly
Use field.
The content of the invention
The present invention proposes a kind of the dilution crystallization technique device and method of the control of film auxiliary, and the membrane module used in method is made
For the scattered interface of dissolved agent, it is uniformly distributed inside membrane module between each film, film side is crystallization solution, and opposite side is dissolved
Agent.By the regulation and control of the conditions such as the solution concentration to film both sides is poor, temperature difference, pressure differential and membrane material, make dissolved agent cross-film
Crystallization solution side is penetrated into, solution is reached degree of supersaturation, produces nucleus.Manipulated using membrane material and operating condition molten
The addition of agent is analysed, so as to control the size distribution and pattern of crystal, the mixed liquor for carrying ideal crystal enters filtration apparatus, obtains
Crystal product to the end.
Technical scheme：
A kind of dilution crystallization device of film auxiliary control, agitating device is installed in the head tank equipped with crystallization solution, former
Batch can chuck connects temperature control device by water-bath pipeline, and temperature control device is used to control the temperature in head tank, the outlet of head tank
Connected successively by valve, peristaltic pump, flowmeter, thermometer, pressure gauge and membrane module side lower port, membrane module side upper end
Mouth is connected by the c mouths of three-way valve A with external storage tank, and external tank bottom is connected by valve with filtration apparatus, filtering dress
Connection filtrate conduit is put, filtrate conduit is connected with the c mouths of three-way valve B；The b that membrane module side upper port passes through three-way valve A
Mouth is connected with three-way valve B, is connected by a mouths of three-way valve B with head tank；Install and stir on the material liquid tank equipped with dissolved agent
Device is mixed, material liquid tank chuck is connected temperature control device with by water-bath pipeline, and temperature control device is used to control the temperature in material liquid tank；Material
Flow container outlet is connected by valve, peristaltic pump, flowmeter, pressure gauge, thermometer with membrane module lower port, membrane module upper port
Material liquid tank is directly connected to, forms the circulating system of dissolved agent；Material liquid tank is placed in precision electronic balance, precision electronic balance connection
Computer, easy to monitor the addition of dissolved agent in real time.
The membrane module is cylindrical, and there is pipe nozzle in the upper and lower part of its shell both ends and shell side,
The film of even distribution is fixed in membrane module.Wherein, for hollow fiber film assembly, it is desirable to which hollow-fibre membrane is in assembly along axis
To arranged in parallel, packing density is between 0.1-0.6；For plate film assembly, ensure that plate membrane assembles smooth, zero defect, nothing
Fold.It is as smooth as possible inside membrane module, the dead bands such as acute angle, right angle are avoided the occurrence of, ensure the size distribution of crystal product
And quality.
A kind of dilution crystallization method of film auxiliary control, step are as follows：
(1) solution to be crystallized is prepared：Prepare mixed solution or solute, the solvent and dissolved agent three of both solute and solvent
Mixed solution, wherein, the addition of dissolved agent does not cause the hypersaturated state of solution in the mixed solution of three, and approaches
Saturation point；
(2) in the mixed solution injection head tank obtained step (1), temperature control device and agitating device is opened, is maintained
30min, makes mixed solution stable homogeneous；
(3) dissolved agent is injected in material liquid tank, opens temperature control device and agitating device, at the same open precision electronic balance and
Computer, maintains 30min, is heated evenly dissolved agent, and balance registration is stablized；
(4) peristaltic pump of control material liquid tank is opened, flow is adjusted, dissolved agent is rapidly injected membrane module, flow through film at a high speed
Side, flow out membrane module afterwards, back in material liquid tank, form dissolved agent circulating system；
(5) treat that dissolved agent circulating system is stable, open the peristaltic pump being connected with head tank, adjust flow, ensure former
The flow velocity of batch can side is 1-10 times of the flow velocity of material liquid tank side；
(6) solution to be crystallized is contacted with dissolved agent in membrane module, reaches supersaturation, produces nucleus.
If continuous operation, carries out crystal growth in membrane module, feed side mixed solution carries crystal in membrane module, from oozing
Membrane module is flowed out in remaining side, flows into external storage tank by three-way valve A, is filtered according to production requirement inflow filter,
Other subsequent treatments are carried out again；Filtrate after filtering returns to secondary profit in head tank by three-way valve A and three-way valve B
With, add solute ensure head tank in solution concentration it is constant.
If intermittently operated, the feed side mixed solution in membrane module flows out membrane module from retentate side, passes sequentially through triple valve
Door A and three-way valve B is flowed back in head tank, is recycled to solution in head tank and is reached supersaturation, carries out crystal growth, treat all molten
Matter is filtered after separating out, filtrate secondary use.
The membrane module is hollow-fibre membrane or plate membrane；Organic film can be used, such as PTFE (polytetrafluoroethylene (PTFE)), PVDF
(Kynoar), PES (polyether sulfone), PVA (polyvinyl alcohol), PAA (polyacrylic acid) etc.；Composite membrane, such as polyvinyl alcohol/micro- sodium
Cellulose, PVA/PAN etc.；Inoranic membrane, such as ceramic membrane, zeolite membrane, metal oxide film, NaA type molecular screen membranes.
Equipment needs periodic cleaning, and solvent is pumped into membrane module using peristaltic pump, adjusts bath temperature higher than operation temperature
5-30 DEG C of degree, solvent circular flow 30-60min in membrane module, film surfaces externally and internally is cleaned up.
Beneficial effects of the present invention：
(1) dissolved agent is scattered, and degree of supersaturation is homogeneous.In the present invention by the way of film adds dissolved agent, solution and film
There is the contact area of bigger on surface, and dissolved agent penetrates film does not have drop diffusional resistance into solution, reduces degree of supersaturation point
The non-uniform defect of cloth.
(2) narrow particle size distribution, crystalline product quality are high.The present invention controls point of degree of supersaturation by film feed postition
Cloth, makes crystal nucleation, growth in one gently stable environment, there is no the problem of outburst nucleation and diauxic growth, effectively
Control the pattern and size distribution of crystal.
(3) have a wide range of application, operating condition is easily changed, and process control is simple.Crystallization is used as using membrane module in the present invention
Core component, regulate and control material flow by adjusting peristaltic pump, temperature control device, feed type, equipment flowsheet and feedstock direction etc.
Speed, temperature difference, pressure differential, degree of supersaturation etc., are no longer limited to a kind of production requirement and a kind of product.
(4) equipment investment is few, is easy to transform, high-efficiency environment friendly.Membrane module filling rate is high, reduces production cost；Film at the same time
Component is easy to amplify and reduces, extension easy to produce；Product post processing is simple, and the recyclable secondary use of filtrate, is not present
Pollution problem.
The present invention makes full use of the bigger serface of film, with reference to membrane separation technique, is aided in using peristaltic pump, temperature control device etc.
Equipment, systematically regulation and control crystallize production process.The present invention changes dissolved agent feed postition during traditional dilution crystallization, passes through
Rational design to membrane module, obtains preferable crystal product, expands the scope of application of dilution crystallization, for some special crystalline substances
Body, such as the production of easily reunion, tough organic matter, fines and temperature sensitive material are significant.The present invention not only protects
The quality and quantity of product have been demonstrate,proved, and it is more economical efficient, and process units simplification, reduces equipment investment；Appointed condition
It is easily changed, process control and easy to operate, practicality is good；Cumbersome post processing is not required in the recycling of product, and filtrate is recyclable
Recycle, environmental protection is without waste liquid.
Brief description of the drawings
Fig. 1 is the dilution crystallization technique device figure of hollow-fibre membrane auxiliary control.
In figure：1 agitating device；2 temperature control devices；3 membrane modules；4 films；5 material liquid tanks；6 head tanks；7 peristaltic pumps；8 thermometers；
9 pressure gauges；10 flowmeters；11 external storage tanks；12 filtration apparatuses；13 precision electronic balances；14 computers；15 (A) three-way valve A；
15 (B) three-way valve B；16 valves.
Embodiment
Below in conjunction with attached drawing and process regimes, embodiment of the invention is further illustrated.
Embodiment 1
Take PES hollow-fibre membranes that membrane module, filling rate 0.6 is made.Take the NaCl of 80g to add in deionized water, be formulated as
Saturated solution at 25 DEG C.Prepared crystallization solution is added in head tank, opens agitating device.Temperature control device is adjusted to 25
DEG C, recirculated water is opened, maintains operating status 30min.Ethanol in proper amount is added into material liquid tank, temperature control device is opened, is adjusted to 25 DEG C,
Recirculated water, electronic balance and computer are opened, maintains operating status 30min.After temperature stabilization, a, b of three-way valve A, B are opened
Mouthful, c mouthfuls are closed, opens ethanol feed liquid tank valve, adjusting peristaltic pump is 50rpm, ethanol is flowed through membrane module.Ethanol is stable
Afterwards, the valve of head tank is opened, adjusts peristaltic pump, the flow for making NaCl solution is 1 times of ethanol flow, and NaCl solution flows into film
Component.There is trickle NaCl nucleus to produce after circular flow 30min, in head tank, rerun 30min, and NaCl is brilliant in head tank
Nucleus growth is the suitable crystal of granularity, closes peristaltic pump and valve, and mixing liquid filtering drying in head tank is obtained NaCl crystalline substances
Body.Computer records the addition of ethanol in real time.
Embodiment 2
Take PES plate membranes that membrane module is made.The NaCl of 80g is taken to add in deionized water, the saturation being formulated as at 25 DEG C is molten
Liquid, ethanol is slowly added dropwise into the solution, and is sufficiently stirred, and makes solution close to supersaturation, but and not up to supersaturation.It will prepare
Good crystallization solution is added in head tank, opens agitating device.Temperature control device is adjusted to 25 DEG C, opens recirculated water, maintains operation
State 30min.Add ethanol in proper amount into material liquid tank, open temperature control device, be adjusted to 25 DEG C, open recirculated water, electronic balance and
Computer, maintains operating status 30min.After temperature stabilization, a, c mouth of three-way valve A, B are opened, closes b mouthfuls, opens ethanol feed liquid
Tank valve, adjusts peristaltic pump 200rpm, ethanol is passed through membrane module at a high speed.After ethanol is stable, the valve of head tank is opened,
Peristaltic pump is adjusted, the flow of NaCl mixed solutions is higher than 10 times of ethanol, NaCl mixed solutions flow into membrane module.After 5min, film
There is trickle NaCl crystal to produce in component, flowing to membrane module exit with mixed liquor is grown into for suitable size, being flowed into
In storage tank, by being filtered in valve inflow filter.If NaCl crystal growths are inadequate, crystal mixed liquor can be made in storage tank
In stay for some time and carry out growth and refilter.Filtered to be dried to obtain NaCl crystal, filtrate flows into head tank, adds again
NaCl.Computer records the addition of ethanol in real time.
Embodiment 3
Take PTFE hollow-fibre membranes that membrane module, filling rate 0.1 is made.Take 25gL- asparagines to add in deionized water, match somebody with somebody
The saturated solution being made as at 25 DEG C, isopropanol is slowly added dropwise into the solution, and is sufficiently stirred, and makes solution close to supersaturation, but
And not up to supersaturation.Prepared crystallization solution is added in head tank, opens agitating device.Temperature control device is adjusted to 25
DEG C, recirculated water is opened, maintains operating status 30min.Appropriate isopropanol is added into material liquid tank, temperature control device is opened, is adjusted to 25
DEG C, recirculated water, electronic balance and computer are opened, maintains operating status 30min.After temperature stabilization, a of opening three-way valve A, B,
C mouthfuls, b mouthfuls are closed, opens isopropanol feed liquid tank valve, adjusts to wriggle and arrives 200rpm, isopropanol is passed through membrane module at a high speed.Isopropyl
After alcohol is stable, the valve of head tank is opened, peristaltic pump is adjusted, the flow of raw material mixed solution is higher than 10 times of isopropanol,
Raw material mixed solution flows into membrane module.There is trickle altheine crystal to produce after 3min, in membrane module, flowed to mixed liquor
Membrane module exit is grown into for suitable size, being flowed into storage tank, by being filtered in valve inflow filter.If
Altheine crystal growth is inadequate, and crystal mixed liquor can be made to stay for some time in storage tank and carry out growth and refilter.By
Filter is dried to obtain altheine crystal, and filtrate is flowed into head tank again, adds altheine.Computer records isopropanol in real time
Addition.
Claims (4)
1. a kind of dilution crystallization device of film auxiliary control, it is characterised in that agitating device is installed on the original equipped with crystallization solution
In batch can, head tank chuck connects temperature control device by water-bath pipeline, and temperature control device is used to control the temperature in head tank, raw material
The outlet of tank is connected by valve, peristaltic pump, flowmeter, thermometer, pressure gauge and membrane module side lower port successively, membrane module
Side upper port is connected by the c mouths of three-way valve A with external storage tank, and external tank bottom connects by valve and filtration apparatus
Connect, filtration apparatus connection filtrate conduit, filtrate conduit is connected with the c mouths of three-way valve B；Membrane module side upper port passes through threeway
The b mouths of valve A are connected with three-way valve B, are connected by a mouths of three-way valve B with head tank；In the material liquid tank equipped with dissolved agent
Upper installation agitating device, material liquid tank chuck are connected temperature control device with by water-bath pipeline, and temperature control device is used to control in material liquid tank
Temperature；Material liquid tank outlet is connected by valve, peristaltic pump, flowmeter, pressure gauge, thermometer with membrane module lower port, film
Component upper port is directly connected to material liquid tank, forms the circulating system of dissolved agent；Material liquid tank is placed in precision electronic balance, accurate electricity
Sub- day flushconnection computer, easy to monitor the addition of dissolved agent in real time.
2. dilution crystallization device according to claim 1, it is characterised in that the membrane module is cylindrical, its shell
There is pipe nozzle in the upper and lower part of both ends and shell side, and equally distributed film is fixed in membrane module；The film group
Part is hollow-fibre membrane or plate membrane, is made of organic film, composite membrane or inoranic membrane.
3. dilution crystallization device according to claim 2, it is characterised in that when membrane module is hollow fiber film assembly,
Hollow-fibre membrane is axially arranged in parallel in membrane module, and packing density is between 0.1-0.6；When membrane module is plate membrane group
During part, ensure that plate membrane assembles smooth, zero defect, corrugationless.
4. with the dilution crystallization method of the dilution crystallization device any one of claim 1-3, it is characterised in that step is such as
Under：
(1) solution to be crystallized is prepared：Prepare the mixed solution or solute of both solute and solvent, solvent and dissolved agent three it is mixed
Solution is closed, wherein, the addition of dissolved agent in the mixed solution of three ensures not causing the hypersaturated state of solution, and approaches
Saturation point；
(2) in the mixed solution injection head tank obtained step (1), temperature control device and agitating device is opened, maintains 30min,
Make mixed solution stable homogeneous；
(3) dissolved agent is injected in material liquid tank, opens temperature control device and agitating device, while open precision electronic balance and electricity
Brain, maintains 30min, is heated evenly dissolved agent, and balance registration is stablized；
(4) peristaltic pump of control material liquid tank is opened, flow is adjusted, dissolved agent is rapidly injected membrane module, flow through the one of film at a high speed
Side, flows out membrane module afterwards, back in material liquid tank, forms the circulating system of dissolved agent；
(5) treat that dissolved agent circulating system is stable, open the peristaltic pump being connected with head tank, adjust flow, ensure head tank
The flow velocity of side is 1-10 times of the flow velocity of material liquid tank side；
(6) solution to be crystallized is contacted with dissolved agent in membrane module, reaches supersaturation, produces nucleus；
If continuous operation, crystal growth is carried out in membrane module, feed side mixed solution carries crystal in membrane module, from retentate side
Membrane module is flowed out, flows into external storage tank by three-way valve A, is filtered according to production requirement inflow filter, then into
Row others subsequent treatment；Filtrate after filtering returns to secondary profit in head tank by three-way valve A and three-way valve B successively
With, add solute ensure head tank in solution concentration it is constant；
If intermittently operated, feed side mixed solution in membrane module flows out membrane module from retentate side, pass sequentially through three-way valve A and
Three-way valve B is flowed back in head tank, is recycled to solution in head tank and is reached supersaturation, carries out crystal growth, treats all solute analysis
Filtered after going out, filtrate secondary use.
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| CN107233744B (en) * | 2017-06-12 | 2019-04-05 | 大连理工大学 | A kind of cooling crystallization method of film auxiliary nucleation |
| CN107320996B (en) * | 2017-08-30 | 2019-03-29 | 哈尔滨工业大学 | A kind of multicomponent mixture film supplement heat rejecter Crystallization Separation method |
| US10675557B2 (en) | 2017-11-03 | 2020-06-09 | Dalian University Of Technology | Continuous crystallization method under control of multistage membrane |
| CN107899266B (en) * | 2017-11-03 | 2019-04-05 | 大连理工大学 | A kind of continuous crystallisation process of Multistage Membranes control |
| CN107890686A (en) * | 2017-12-06 | 2018-04-10 | 大连理工大学 | A kind of high performance membrane dilution crystallization method of double unit coupling cycles |
| CN108499153B (en) * | 2018-03-14 | 2020-06-02 | 山东大学 | Temperature control device and method for high-throughput parallel crystallization instrument |
| CN109794078A (en) * | 2019-03-21 | 2019-05-24 | 大连理工大学 | A kind of method and system of the automatic nucleus screening of membrane interface regulation |
| CN109833641A (en) * | 2019-04-04 | 2019-06-04 | 上海电气集团股份有限公司 | A kind of strong brine crystal system and application method |
| CN115259113A (en) * | 2021-04-29 | 2022-11-01 | 浙江蓝天环保高科技股份有限公司 | Method and device for continuously purifying lithium bis (fluorosulfonyl) imide |
| CN114470851A (en) * | 2022-01-20 | 2022-05-13 | 大连理工大学 | Bionic system and method for in-vitro regulation and control of inorganic salt crystallization |
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| JP5704630B2 (en) * | 2010-06-24 | 2015-04-22 | 日本電信電話株式会社 | Crystallization process control method and apparatus |
| CN102924539B (en) * | 2012-10-31 | 2015-05-20 | 南京工业大学 | Method for preparing trehalose crystals |
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