CN106589099A - Desalination system and desalination method for soluble silk fibroin solution - Google Patents
Desalination system and desalination method for soluble silk fibroin solution Download PDFInfo
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- CN106589099A CN106589099A CN201710059839.6A CN201710059839A CN106589099A CN 106589099 A CN106589099 A CN 106589099A CN 201710059839 A CN201710059839 A CN 201710059839A CN 106589099 A CN106589099 A CN 106589099A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07K—PEPTIDES
- C07K14/00—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof
- C07K14/435—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans
- C07K14/43504—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans from invertebrates
- C07K14/43563—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans from invertebrates from insects
- C07K14/43586—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans from invertebrates from insects from silkworms
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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
- B01D61/58—Multistep processes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/124—Water desalination
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Abstract
The invention discloses a desalination system and a desalination method for a soluble silk fibroin solution. The desalination system comprises a diffusive dialysis module and an electrodialysis module, wherein a liquid outlet of the diffusive dialysis module is connected with an inlet of the electrodialysis module. The desalination method comprises the following steps: introducing a silk fibroin solution into a raw material box of the diffusive dialysis module to perform diffusive dialysis so as to obtain a primary desalination silk fibroin solution; introducing the primary desalination silk fibroin solution into a raw material box of the electrodialysis module to perform electrodialysis so as to obtain a secondary desalination silk fibroin solution. According to the desalination system and the desalination method disclosed by the invention, diffusive dialysis and electrodialysis are combined together, and are applied to desalination in a protein organic system for the first time, the high concentration difference of the silk fibroin solution is fully used, and when the desalination efficiency is relatively high by taking the concentration difference as a driving force, desalination is carried out by using diffusive dialysis; and when the desalination efficiency is relatively low by taking the concentration difference as a driving force, the diffusive dialysis is replaced by electrodialysis in time, and desalination is carried out by taking a potential difference as a driving force, so that not only is low energy consumption ensured but also a high desalination efficiency is ensured.
Description
Technical field
The present invention relates to the processing technology field of protein solution, more particularly to a kind of soluble silk fibroin protein solution it is de-
Salt system and desalination process.
Background technology
Silk (is cladded with and is cohered by the fibroin albumen (core fiber) and 25% sericin for accounting for gross weight 75%
Layer) composition.Fibroin albumen is a kind of application prospect functional material widely, is widely used in clothes, medical science, biology etc.
Field.Natural fibroin albumen is water insoluble, but can be dissolved in strong acid, highly basic and some neutral salt solutions.Due to strong acid it is strong
Alkali can destroy the protein structure of fibroin albumen, and some neutral salt such as chloride and iodide are again harmful, so now most
Conventional is exactly to dissolve fibroin albumen with calcium chloride-ethanol-water Ternary System.
Concentration for salt in the ternary system for dissolving fibroin albumen is high, and desalination becomes in soluble fibroin albumen production
Important step.Most traditional desalination process uses bag filter desalination, and time-consuming for the method, and batch is few, costly.With film
The membrane technologies such as the development of engineering, ultrafiltration, nanofiltration, electrodialysis are increasingly being used for desalination.
Notification number removes fibroin albumen to adopt nanofiltration in the patent application of CN1392265A and CN102172257A
High salt concentration in solution, salt rejection rate is respectively 98% and 90%.Notification number for CN101381758A patent application in adopt
Ultrafiltration and nanofiltration combination desalination：First the macromolecular peptide fragment in solution is separated with hyperfiltration technique, then separated using nanofiltration highly concentrated
The salt of degree, salt rejection rate is less than 93.5%.Though above method can shorten the desalination time than traditional bag filter desalination, due to super
That filter and nanofiltration are utilized is fibroin albumen and CaCl2The difference of molecular weight is separated both, so salt rejection rate is not high, and
It is all pressure differential to separate relied on motive force, and as salt content is gradually lowered in silk fibroin protein solution, desalting efficiency also can be by
Gradually reduce, desalination time lengthening, to the later stage of desalination, desalting efficiency can become lower.In addition, the film that nanofiltration and ultrafiltration are used
Aperture is very little, and film surface is very fine and close, and the solution viscosity after fibroin albumen dissolving is larger, can cause the blocking of film runner, real
When border is applied, NF membrane needs Jing often to clean, and so as to reduce desalting efficiency, extends the desalination time.
Notification number finally gives to prepare a kind of SP using electrodialysis desalination in the patent application of CN103897021A
Total heteroion content is less than 1% in SP.Notification number for CN103243145A patent application in first with electrodialysis desalination, then
Using dialysis bag filtration, final salt rejection rate is 99.5%.Though the desalination time is substantially shorter using electrodialysis desalination, while also may be used
Salt rejection rate is set to reach close 100%.But CaCl in the silk fibroin protein solution at initial stage2Concentration reached 400g/L, if using
Electrodialytic technique makes salt rejection rate reach 99.5%, and its energy consumption is very high.Moreover, electrodialysis desalination is all needed from start to finish
Electric energy is consumed, in fact, there is so high concentration difference between solution and deionized water, is started to considerably long one section from desalination
Desalination can be carried out in time as motive force by the use of concentration difference completely, it is not necessary that consume electric energy.Generally, before desalination
CaCl in silk fibroin protein solution2Concentration all in 150g/L-300g/L, with electrodialytic technique come desalination, desalination not only occurs
Rate is low, energy consumption is big, desalination overlong time the problems such as, but also there is electrodialysis plant needs high current to run, and easily damages
The dangerous situations such as bad electric leakage.
The content of the invention
The purpose of the present invention is for technological deficiency, first aspect present in prior art, there is provided a kind of salt rejection rate height
And the desalination system of the soluble silk fibroin protein solution of energy-conservation, including material box, diffusion dialysis module and electrodialysis module, raw material
Case has two imports of the import of diffusion dialysis liquid and electrodialysis material inlet, and material outlet and electrodialysis material outlet two go out
Mouthful, wherein, the diffusion dialysis liquid import of material box and material outlet are connected with diffusion dialysis module, the electrodialysis raw material of material box
Import and electrodialysis material outlet are connected with electrodialysis module.
The diffusion dialysis module includes diffusion dialysis material pump, diffusion water pump, diffusion dialysis device and deionization water tank；Diffusion
Dialyzer is connected by diffusion dialysis material pump with material box, and deionization water tank is connected by diffusion water pump with diffusion dialysis device.
The diffusion dialysis device is provided with material inlet, the outlet of diffusion dialysis liquid, diffusion water inlet and diffusion water out；Raw material
Import and the outlet of diffusion dialysis liquid are connected respectively with the material outlet of material box and diffusion dialysis liquid import；Diffusion water inlet and expansion
Aproll outlet is connected respectively with the water out and water inlet of deionization water tank；Preferably, material inlet in the diffusion dialysis device
Diagonal is taken to arrange with the position of diffusion dialysis liquid outlet；Also diagonal is taken in the position of diffusion water inlet and diffusion water out
Arrange.
Material flow meter and feed pressure table are additionally provided with pipeline between the material box and diffusion dialysis device；It is described to go
Divergent flow gauge and diffusion water pressure table are additionally provided with pipeline between ionized water tank and diffusion dialysis device.
The electrodialysis module includes electric osmose analysis of material pump, electrodialysis water pump, electric dialyzator and water tank；Electric dialyzator is by electricity
Dialysis material pump is connected with material box, and water tank is connected by electrodialysis water pump with electric dialyzator.
The electric dialyzator includes the enriched chamber of longitudinal alternating parallel arrangement and diluting compartment, and the electrodialysis of the material box is former
Material import is connected with diluting compartment outlet；The electrodialysis material outlet of material box is connected with enriched chamber's import；Diluting compartment import and dense
The outlet of contracting room is connected respectively with the water outlet of water tank and concentrated water import.
A desalting soln flowmeter is additionally provided with pipeline between the material box and electric dialyzator and a desalination is molten
Hydraulic coupling table；Electrodialytic water flowmeter and electrodialytic water pressure gauge are additionally provided with pipeline between the water tank and electric dialyzator.
Second aspect, the present invention provides a kind of desalination process of soluble silk fibroin protein solution, using above-mentioned desalination system,
By silk fibroin protein solution by being passed through in material box in diffusion dialysis module, dialysis is diffused, obtains a desalination fibroin albumen
Solution；A desalination silk fibroin protein solution is passed through in the material box of electrodialysis module again carry out electrodialysis, obtains secondary desalination
The silk fibroin protein solution that silk fibroin protein solution, i.e. desalination are completed.
Comprise the following steps：
(1), a desalination is carried out using diffusion dialysis：Open diffusion dialysis mould fast, electrodialysis module is closed, in material box
Silk fibroin protein solution (silk fibroin protein solution is by silk through Na2CO3Degumming, calcium chloride-ethanol-water Ternary System dissolving system
) entered from the material inlet of diffusion dialysis device according to liquid linear velocity 1-5cm/s by diffusion dialysis material pump, ooze through diffusion
Export out from diffusion dialysis liquid after analysis, circulation flow back in material box, diffusion water pump by the deionized water in deionization water tank with
Linear velocity 1-5cm/s flows out from diffusion water inlet suction diffusion dialysis device from diffusion water out, and recycle stream is gone back ionized water tank
In；When the salt content of deionized water in deionization water tank is 60-70% (preferably 65%) of initial salt content, stops diffusion and ooze
Analysis, obtains a desalination silk fibroin protein solution；The linear velocity ratio of silk fibroin protein solution and deionized water is (1-2)：1, (preferably 2：
1)；
(2), secondary desalination is carried out using electrodialysis：Close diffusion dialysis mould fast, open electrodialysis module, switch on power
(electric current be less than 0.3A, preferred 0.2A), electric osmose analysis of material pump is with liquid linear velocity 1-5cm/s by a desalination silk in material box
The diluting compartment of fibroin solution Jing electrodialysis liquid import suction electric dialyzators, Jing after electrodialysis desalination, from the electrodialysis of diluting compartment
Products export flows out, and circulation is flowed in material box, while by the deionized water in water tank with liquid linear velocity 1-5cm/s from electric osmose
The water outlet of parser enters enriched chamber, carries out after ion exchange with a desalination silk fibroin protein solution, and the outlet from enriched chamber is flowed
Go out, circulation is flowed in water tank；When the electrical conductivity of silk fibroin protein solution in material box is below 200 μ S/cm, stop electrodialysis,
Secondary desalination silk fibroin protein solution is obtained, i.e., the silk fibroin protein solution that desalination is completed is derived by electrodialysed product outlet；
Preferably, in material box before diffusion dialysis the concentration of silk fibroin protein solution in below 6wt%, diffusion dialysis device
Block board thickness is 2mm-3mm, and the block board thickness of diluting compartment is 2mm-3mm in electric dialyzator, and the block board thickness of enriched chamber is
0.5mm；Preferably, the ion exchange resin filled in diluting compartment is by anion exchange resin and cationic ion-exchange resin quality
Than for 1:1-1:1.5 hybrid resins for obtaining.
The third aspect, the present invention provides a kind of production method of soluble fibroin albumen, takes silk Na2CO3Degumming, chlorine
Change calcium-ethanol-water Ternary System dissolving and obtain silk fibroin protein solution, then desalination process described in Jing claims 8 or 9 to fibroin egg
White solution carries out desalination, obtains secondary desalination silk fibroin protein solution, finally carries out freeze-drying, that is, obtain fibroin albumen.
Compared with prior art, the invention has the beneficial effects as follows：
(1) desalination system of the invention and desalination process by diffusion dialysis in combination with electrodialysis, first for protein
Desalination in organic system, makes full use of the concentration difference of silk fibroin protein solution itself, with concentration difference as motive force desalting efficiency
When higher, using diffusion dialysis desalination is carried out；When relatively low as motive force desalting efficiency with concentration difference, replaced with electrodialysis in time
Diffusion dialysis, by motive force of potential difference desalination is carried out, and both ensure that low energy consumption in turn ensure that high desalination efficiency.
(2) present invention in diffusion dialysis, using reflux type run, and can increase contact surface by solution and deionized water
Product, improves desalting efficiency.
(3) deionized water can be recycled within the specific limits in the present invention, when change in the TDS value unit interval of solution
Water is changed when changing slower, water consume is reduced to greatest extent.
Description of the drawings
Fig. 1 show the principle schematic of diffusion dialysis desalination in desalination system of the present invention；
Fig. 2 show the structural representation of desalination system of the present invention；
Fig. 3 show the structural representation of desalination system another embodiment of the present invention.
Specific embodiment
The invention provides the desalination system and desalination process of a kind of soluble silk fibroin protein solution, i.e., integrated diffusion dialysis
Module and electrodialysis module carry out desalination.The present invention takes full advantage of the concentration difference of silk fibroin protein solution itself, first with expansion
Scattered dialysis carries out primary desalination, after the salinity in silk fibroin protein solution is reduced to a certain extent, then with electrodialysis desalination, fills
Both respective technical advantages have been waved in distribution, so both reduced initial stage concentration larger solution and electric dialyzator intermediate ion is exchanged
The infringement of film, reduces the electric energy consumed required for this part again, not only efficient but also energy-conservation.Because diffusion dialysis is using diffusion
The concentration difference of dialyser both sides solution realizes desalination for motive force；Electrodialysis is then to pass through ion in the presence of extra electric field
Displacement desalination, the two combines and carries out desalination to silk fibroin protein solution, gives full play to the advantage of the two, both can realize high de-
Salt efficiency, equipment with high desalinization, may insure desalination processes safety again.Wherein,
Diffusion dialysis as a kind of membrane separation technique with concentration difference as motive force, with simple to operate, low energy consumption, without two
The advantages such as secondary pollution.But diffusion dialysis at present is frequently utilized for reclaiming the spent acid and salkali waste in inorganic waste liquids, molten for fibroin albumen
The desalination of liquid has not been reported.This is because the principle of diffusion dialysis is the competitive diffusion of ion, i.e.,：In waste acid recovery, H+Easily water side is reached through cavity block than other metal cations, realize the separation of acid；When salkali waste is reclaimed, OH-Than other acid
Radical ion easily reaches water side through film, realizes the separation of alkali.It can be seen that, diffusion dialysis is due to H+And OH-With other ions it
Between there is emulative separation, it is easier to reach water side through film, so currently used for waste acid recovery and salkali waste, and have no for
Desalination.
Then using diffusion dialysis desalination is carried out in the present invention, its core is at 2 points：One is diffusion dialysis film both sides solution
Concentration difference；Two is the selective penetrated property of diffusion dialysis film.If as shown in figure 1, the diffusion dialysis film in diffusion dialysis module
For cation-exchange membrane, then Ca is only allowed2+Pass through, due to the concentration difference that the principle of charge conservation in solution and film both sides are larger,
Cl-Can be with Ca2+Diffusion and be gradually diffused into the opposite side of film, so as to reach the purpose of desalination.In order to effective in the present invention
The desalination of silk fibroin protein solution is carried out, the high viscosity of silk fibroin protein solution is specifically designed for, is innovatively proposed in diffusion dialysis device
Some dividing plates, and the filling male ion-exchange resin in the compartment being made up of dividing plate are set, and the ion in such solution is in resin
Upper diffusion velocity is fast than in aqueous, and resin can also play good stirring action in runner so that the thickness of liquid film
Degree is thinning, and the resistance of ion diffusion is substantially reduced, so as to improve desalting efficiency.Also, also determine dividing plate by a large amount of explorations
Thickness be 2-3mm, and the double-edged fine-toothed comb for preventing resin leakage is provided with diffusion dialysis device two ends.
Notification number is used for two sections of diffusion dialysis, two sections of electrodialysis and Bipolar Membrane used in the patent application of CN105645644A
Sulfuric acid in reclaim sulfuric acid and sodium sulfate wastewater；Notification number for CN103362010A patent application in propose a kind of pulp
The diffusion dialysis pretreating process of the Black Liquor by Electrodialysis alkali collection in manufacture, is pre-processed black liquor using diffusion dialysis, is obtained
Electrodialysis process is reused to after sig water；Notification number for CN103349912A patent application in be equally to use diffusion dialysis
First pre-processed, the alkali in then recycling electrodialysis to reclaim viscose fiber production process in produced waste liquid.With top
Method is to be combined diffusion dialysis and electrodialysis, reclaims spent acid and salkali waste in inorganic system, but is being contained respectively without being applied
Report in the protein solution of amino acid and peptide chain.This is because, inorganic system viscosity is less, impurities are more single,
Diffusion dialysis and electrodialysis are combined, are only suitable for inorganic system or Acid-Base System.It is contained miscellaneous and silk fibroin protein solution viscosity is larger
Matter situation is more complicated, while fouling membrane situation is more serious, directly above diffusion dialysis and electrodialysis GC-MS to be used for into fibroin
The desalination of protein solution, has that high cost, desalting efficiency are low, change film frequency.Therefore, in order to overcome fibroin albumen
The high viscosity problem of solution, arranges some dividing plates in electric dialyzator, the compartment being made up of dividing plate define some enriched chambers and
Some diluting compartments, and the filling ion-exchange resin in diluting compartment, the ion exchange resin of filling is by anion exchange resin
It is 1 with cationic ion-exchange resin mass ratio:(1-1.5) hybrid resin for obtaining, this electrodialysis is referred to as packed-bed electrodialysis.In electricity
Under the DC electric field effect of dialysis, the salt ion in silk fibroin protein solution can realize that ion is quick by ion exchange resin
Migration, because migration velocity of the ion on resin is than the fast 2-3 order of magnitude in the solution；The filling of resin, in runner
Good stirring action can be played so that the thickness of liquid film is thinning, the resistance of Ion transfer is substantially reduced.Also, also pass through
It is 2-3mm that a large amount of explorations determine the thickness of diluting compartment dividing plate, and the thickness of enriched chamber's dividing plate is 0.5mm, and in electric dialyzator
Two ends are provided with the double-edged fine-toothed comb for preventing resin leakage.
Inventor explores a set of process conditions through long-term practice and substantial amounts of experiment, by diffusion dialysis and electric osmose
Analysis conjunctive use not only increases desalting efficiency in the desalination processes of protein solution, also largely reduces energy consumption.
Below in conjunction with specific embodiment, present disclosure is further illustrated, and the present invention is further elaborated, but
These embodiments limit the invention absolutely not.
The desalination system of soluble silk fibroin protein solution proposed by the present invention, including diffusion dialysis module, electrodialysis module
With material box 10, as shown in Fig. 2 diffusion dialysis module shares a material box 10 with electrodialysis module, material box has two to enter
Mouthful (import of diffusion dialysis liquid and electrodialysis material inlet), two outlets (material outlet and electrodialysis material outlet), import and
Outlet is communicated inside material box, and diffusion dialysis module and electrodialysis module are coupled together.
Diffusion dialysis module, as shown in Fig. 2 including diffusion dialysis material pump 2, diffusion dialysis device 5 and deionization water tank 9.Its
In, diffusion dialysis device 5 is provided with material inlet, the outlet of diffusion dialysis liquid, diffusion water inlet and diffusion water out；Material inlet and expansion
The outlet of scattered dialysate is connected respectively with the material outlet of material box 10 and diffusion dialysis liquid import；Diffusion water inlet and diffusion water go out
Mouth is connected respectively with the water out and water inlet of deionization water tank 9.The dividing plate of some vertical placements is set in diffusion dialysis device 5,
Diffusion dialysis device inner space is separated out in several compartments, compartment and is filled with cationic ion-exchange resin by dividing plate；Cation exchange
Resin is polystyrene gel type resin.The position of material inlet and the outlet of diffusion dialysis liquid takes right in diffusion dialysis device 5
Linea angulata is arranged；Also diagonal is taken to arrange in the position of diffusion water inlet and diffusion water out；So that the diffusion in diffusion dialysis device 5
Water and raw material reverse flow, increase contact area, improve desalting efficiency and salt rejection rate.Soluble fibroin is contained with material box 10
Protein solution, the material outlet of material box 10 is connected by diffusion dialysis material pump 2 with the material inlet of diffusion dialysis device 5, by original
Soluble silk fibroin protein solution in hopper 10 is pumped into and carry out in diffusion dialysis device 5 desalination.Diffusion dialysis material pump 2 and diffusion
Material flow meter 3 and feed pressure table 4 are additionally provided with pipeline between dialyzer 5.Meanwhile, it is contained with deionization water tank 9
Ionized water, the water out of deionization water tank 9 is connected by diffusion water pump 8 with the diffusion water inlet of diffusion dialysis device 5, by deionization
Water is pumped in diffusion dialysis device 5.Pipeline between deionization water tank 9 and diffusion dialysis device 5 is provided with divergent flow gauge 7 and expands
Aproll pressure gauge 6.After raw material silk fibroin protein solution in diffusion dialysis device 5 is contacted with diffusion water, the salt in raw material diffuses to water
In, being removed, salinity is reduced in raw material, becomes diffusion dialysis liquid, and salinity is raised in deionized water, becomes diffusion water,
Diffusion dialysis liquid again Jing diffusion dialysis device 5 diffusion dialysis liquid outlet be connected with the diffusion dialysis liquid import of material box 10, return
Into material box 10, the diffusion water out for spreading water Jing diffusion dialysis device 5 again is back in deionization water tank 9, is completed diffusion and is oozed
Analysis desalination.So circulation, the 60%- of salt content before the salt content in deionization water tank 9 reaches silk fibroin protein solution desalination
When 70%, terminate diffusion dialysis circulation, the diffusion dialysis liquid (a desalination silk fibroin protein solution i.e. after desalination) is imported into electricity
Dialysis module.
Electrodialysis module, as shown in Fig. 2 including electric osmose analysis of material pump 11, electric dialyzator and water tank 18.The electric osmose of material box 10
Analysis material inlet is exported with the electrodialysed product of electric dialyzator 1 and the outlet of diffusion dialysis liquid is connected；The electrodialysis of material box 10 is former
Material outlet is connected with the electrodialysis liquid import of electric dialyzator 1.The dividing plate of some vertical placements is provided with electric dialyzator 1, dividing plate will
The inner space of electric dialyzator 1 is separated in some compartments, compartment alternately filled with anion exchange resin and cation exchange
Resin, therefore each compartment defines enriched chamber and the diluting compartment of parallel longitudinal arrangement, the bottom right of electric dialyzator 1 and upper left are distinguished
There are fresh water import and electrodialysed product outlet, there are respectively the import of electrodialysis liquid and concentrated water outlet in the upper right of electric dialyzator 1 and lower-left.
Anion exchange resin can be polystyrene series anion exchange resin, and cationic ion-exchange resin can be polystyrene sun
Ion exchange resin.Fresh water import and concentrated water outlet are connected respectively with the water outlet of water tank 18 and concentrated water import.Material box 10
In hold a desalination silk fibroin protein solution Jing after diffusion dialysis desalination, the electrodialysis material outlet of material box 10 passes through electric osmose
Analysis of material pump 11 is connected with the electrodialysis material inlet of electric dialyzator 1, by a desalination silk fibroin protein solution pump in material box 10
Enter and carry out in electric dialyzator 1 secondary desalination.A desalination is additionally provided with pipeline between electric osmose analysis of material pump 11 and electric dialyzator 1 molten
Flow meters 12 and a desalting soln pressure gauge 13.Meanwhile, deionized water, the water outlet of water tank 18 are contained with water tank 18
It is connected with the fresh water import of electric dialyzator 1 by electrodialysis water pump 17, deionized water is pumped in the diluting compartment of electric dialyzator 1.
Pipeline between water tank 9 and electric dialyzator 1 is provided with electrodialytic water flowmeter 16 and electrodialytic water pressure gauge 15.Electric dialyzator 1
In desalination silk fibroin protein solution and fresh water into contact after, the salt in solution is diffused in water, is removed, and salt is dense in solution
Degree is reduced, and becomes electrodialysed product, and salinity is raised in fresh water, becomes concentrated water, the electric osmose of electrodialysed product Jing electric dialyzators 1 again
Analysis products export be back in material box 10, concentrated water again Jing electric dialyzators 1 concentrated water outlet be back in water tank 18, complete electric osmose
Analysis desalination, when the electrical conductivity of solution in material box 10 is down to below 200 μ S/cm, by electrodialysed product (i.e. secondary desalination fibroin
Protein solution) drawn by electrodialysed product outlet, then it is freeze-dried, obtain final product solid silk fibroin powder.
In order to shorten the desalination time, above desalination system can be improved, as shown in figure 3, being only diffusion dialysis module
Material box 10 is no longer shared with electrodialysis module, and is divided into diffusion dialysis material box 19 and electrodialysis material box 20.Wherein, expand
The liquid outlet of scattered dialysis material box arranges a threeway, or being connected with the material inlet of diffusion dialysis device, or and electrodialysis
The electrodialysis material inlet of material box is connected.Remaining structure is and annexation is identical with the system shown in Fig. 2.
Based on the desalination system of the soluble silk fibroin protein solution shown in figure 2 above, present invention also offers a kind of solvable
The desalination process of property silk fibroin protein solution, comprises the following steps：
(1), a desalination is carried out using diffusion dialysis：Electrodialysis module is closed, it is first that the fibroin albumen in material box is molten
(silk is through Na for liquid2CO3Degumming, calcium chloride-ethanol-water Ternary System dissolving is obtained) pass through diffusion dialysis material pump 2 according to liquid
Linear velocity 1-5cm/s is entered from the material inlet of diffusion dialysis device, exports out from diffusion dialysis liquid after dialysis, recycle stream
In returning material box, diffusion water pump 8 is by the deionized water in deionization water tank with the expansion of linear velocity 1-5cm/s suction diffusion dialysis device
Aproll import, flows out from diffusion water out, in circulation reflow tank.When salt content reaches silk fibroin protein solution in deionization water tank
Stop diffusion dialysis during 60%-70% (preferably 65%) of salt content before desalination, it is molten for a desalination fibroin albumen in material box
Liquid.
The linear velocity ratio of silk fibroin protein solution and deionized water is (1-2):1 (preferably 2：1), the flow velocity in diffusion dialysis
(i.e. linear velocity) affects the diffusion velocity of ion, and flow velocity is faster, the speed in calcium ion and chlorine ion binding capacity to deionized water
It is faster.
(2), secondary desalination is carried out using electrodialysis：Diffusion dialysis module is now closed, electrodialysis module is opened, in electric osmose
Parser electrode both sides are passed through 0.1g/LNa2SO4Solution (pole water), switches on power, and electric current is below 0.3A (preferred 0.2A).Electricity consumption
A desalination silk fibroin protein solution in material box is passed through electricity by dialysis material pump 11 by flexible pipe according to liquid linear velocity 1-5cm/s
The electrodialysis liquid import of dialyzer 1 enters electric dialyzator 1, Jing after electrodialysis desalination, flows out from electrodialysed product outlet, recycle stream
In entering material box, while by the deionized water in water tank according to liquid linear velocity 1-5cm/s from water outlet suction electric dialyzator 1
In, carry out after ion exchange with a desalination silk fibroin protein solution, to flow out from concentrated water outlet, circulation is flowed in water tank.Work as raw material
When silk fibroin protein solution electrical conductivity is not higher than 200 μ S/cm in case, stop electrodialysis, be now secondary desalination fibroin in material box
Protein solution, it is derived to subsequent processing by electrodialysed product outlet.
(3), freeze-drying：By secondary desalination silk fibroin protein solution first in -80 DEG C of precoolings to there is no liquid fibroin albumen,
Carry out freeze-drying under vacuum again, that is, obtain solid filament fibroin.
Wherein start before desalination, the weight/mass percentage composition of fibroin albumen is selected in silk fibroin protein solution in material box
Below 6wt%, in order to ensure the flowing of good solution and the migration of salt ion and diffusion, while reducing the pressure to film
Power.Diffusion dialysis device median septum thickness is that between 2mm-3mm, cation-exchange membrane adopts homogeneous and heterogeneous.Diffusion
Dialysis process salt rejection rate can flexibly be controlled and adjusted by its run time, when a salt rejection rate reaches 60%-70%, then
Desalination silk fibroin protein solution is introduced in electrodialysis module to be carried out secondary desalination no longer reduces to salt content, certain
In the range of, the time shorter (0.2A is optimum) of the secondary desalination of the bigger electrodialysis of electric current.
Embodiment 1
1) according to Na2CO3Concentration is 5g/L, and bath raio is 1：40, degumming is carried out to silk.
The sodium carbonate of 20g is added in 4000ml running water, then silk boiling in water is put into into and is boiled 30min, change weight after liquid
30min is boiled again, 30min is boiled with the deionized water boiling for adding sodium carbonate for the third time, and after every 30min picric acid cochineal solution is used
Whether inspection silk gum takes off.Then deionized water is cleaned, 50 DEG C of drying, is cut into segment, standby.
2) it is 1 according to mol ratio：2：8 prepare calcium chloride-ethanol-water Ternary System solution, and silk is dissolved.
490ml deionized waters are added in there-necked flask, 377.4gCaCl is then slowly added into2, CaCl is added in water2Meeting
Substantial amounts of heat is produced, until temperature drops to 60 DEG C or so, there-necked flask is put in 60 DEG C of water-baths, measured with graduated cylinder
395ml absolute ethyl alcohols are poured slowly in flask, and then the silk segment for shearing is added in lysate, when silk it is all molten
Xie Hou, continues agitating heating dissolving 4h.After dissolving, treat that silk fibroin protein solution is cooled to room temperature, then use centrifuge 8000r/
Min, is centrifuged 10min, takes supernatant and is fitted into standby in bottle.
The technical parameter of diffusion dialysis module
Appearance and size：100mm×200mm；Effective dimensions：70mm×120mm；Block board thickness：2-3mm；Diffusion dialysis sun
Film：Fine and close homogeneous phase cation exchange film；Film logarithm 10 pairs
The technical parameter of electrodialysis membrane stack
Appearance and size：100mm×200mm；Effective dimensions：70mm×120mm；Enriched chamber's block board thickness：0.5mm, desalination
Room block board thickness 2-3mm；Homogeneous phase anion/cation exchange membrane：Fine and close homogeneous phase anion/cation exchange membrane；Film logarithm 10 pairs.
120g steps 2 are taken in material box) in obtained silk fibroin protein solution, add the water of 100ml, concentration dilution is extremely
4%, 2000ml deionized waters are added in deionization water tank, it is 40L/h to adjust silk fibroin protein solution flow, and the flow of water is 20L/
H, is circulated desalination, after 6.8h to salt rejection rate be 65% when, it is out of service.
The silk fibroin protein solution after a desalination is taken, adds 2000ml deionized waters to carry out electrodialysis in water tank secondary de-
Salt, it is 40L/h to adjust silk fibroin protein solution flow, and the flow of water is 20L/h, is passed through pole water, and the flow for adjusting pole water is 3L/h,
After waterflow stabilization, dc source is connected, regulation electric current is 0.2A, when the electrical conductivity of electrodialysed product reaches 200 μ S/cm (i.e.
TDS is 0.1g/L) left and right when stop desalination, the desalination time is 3.5h, and final salt rejection rate is 99.98%, the fibroin albumen rate of recovery
For 91.35%, calculate power consumption and be less than 0.0175KWh.
Silk fibroin protein solution in following examples is using step 1 in embodiment 1) and it is 2) prepared；Diffusion dialysis mould
The technical parameter of block and electrodialysis module is also same as Example 1.
Embodiment 2
Take 120g silk fibroin protein solutions in material box, add the deionized water of 100ml, concentration dilution to 4%, go from
2000ml deionized waters are added in sub- water tank, it is 40L/h to control silk fibroin protein solution flow, and the flow of water is 20L/h, is expanded
Desalination of scattered dialysis, after 6h to salt rejection rate be 60% when, it is out of service.
A desalination silk fibroin protein solution is taken, adds 2000ml deionized waters to carry out the secondary desalination of electrodialysis in water tank, adjusted
It is 40L/h to save silk fibroin protein solution flow, and the flow of water is 20L/h, is passed through pole water, and the flow for adjusting pole water is 3L/h, is circulated
After waterflow stabilization, connection dc source, control electric current 0.2A, when silk fibroin protein solution electrical conductivity reaches 200 μ S/cm, (i.e. TDS is
0.1g/L) stop desalination during left and right, measure the desalination time for 3.8h.Final salt rejection rate is 99.92%, and the fibroin albumen rate of recovery is
91.0%, power consumption is less than 0.02KWh.
Embodiment 3
Take 120g silk fibroin protein solutions in material box, add the deionized water of 100ml, concentration dilution to 4%, go from
2000ml deionized waters are added in sub- water tank, it is 40L/h to control silk fibroin protein solution flow, and the flow of water is 20L/h, is expanded
Desalination of scattered dialysis, after 8h to salt rejection rate be 70% when, it is out of service.
A desalination silk fibroin protein solution is taken, adds 2000ml deionized waters to carry out the secondary desalination of electrodialysis in water tank, adjusted
It is 40L/h to save silk fibroin protein solution flow, and the flow of water is 20L/h, is passed through pole water, and the flow for adjusting pole water is 3L/h, is circulated
After waterflow stabilization, connection dc source, control electric current 0.2A, when silk fibroin protein solution electrical conductivity reaches 200 μ S/cm, (i.e. TDS is
0.1g/L) stop desalination during left and right, measure the desalination time for 3h.Final salt rejection rate is 99.89%, and the fibroin albumen rate of recovery is
88.24%, power consumption is less than 0.015KWh.
Embodiment 4
Take 120g silk fibroin protein solutions in material box, add the deionized water of 100ml, concentration dilution to 4%, go from
2000ml deionized waters are added in sub- water tank, it is 20L/h to control silk fibroin protein solution flow, and the flow of water is 40L/h, is expanded
Desalination of scattered dialysis, after 11.5h to salt rejection rate be 65% when, it is out of service.
A desalination silk fibroin protein solution is taken, adds 2000ml deionized waters to carry out the secondary desalination of electrodialysis in water tank, adjusted
It is 20L/h to save silk fibroin protein solution flow, and the flow of water is 40L/h, is passed through pole water, and the flow for adjusting pole water is 3L/h, is circulated
After waterflow stabilization, dc source, control voltage 25V, electric current 0.2A, when silk fibroin protein solution electrical conductivity reaches 200 μ S/cm are connected
Stop desalination during (i.e. TDS is 0.1g/L) left and right, measure the desalination time for 4.5h.Final salt rejection rate is 99.90%, fibroin albumen
The rate of recovery is 83.74%, and power consumption is less than 0.225KWh.
Embodiment 5
Take 120g silk fibroin protein solutions in material box, add the deionized water of 100ml, concentration dilution to 4%, go from
2000ml deionized waters are added in sub- water tank, it is 20L/h to control silk fibroin protein solution flow, and the flow of water is 20L/h, is expanded
Desalination of scattered dialysis, after 8h to salt rejection rate be 65% when, it is out of service.
A desalination silk fibroin protein solution is taken, adds 2000ml deionized waters to carry out the secondary desalination of electrodialysis in water tank, adjusted
It is 20L/h to save silk fibroin protein solution flow, and the flow of water is 20L/h, is passed through pole water, and the flow for adjusting pole water is 3L/h, is circulated
After waterflow stabilization, dc source, control voltage 25V, electric current 0.2A, when silk fibroin protein solution electrical conductivity reaches 200 μ S/cm are connected
Stop desalination during (i.e. TDS is 0.1g/L) left and right, measure the desalination time for 4h.Final salt rejection rate is 99.94%, and fibroin albumen is returned
Yield is 90.42%, and power consumption is less than 0.2KWh.
Embodiment 6
Take 120g silk fibroin protein solutions in material box, add the deionized water of 100ml, concentration dilution to 4%, go from
2000ml deionized waters are added in sub- water tank, it is 40L/h to control silk fibroin protein solution flow, and the flow of water is 20L/h, is expanded
Desalination of scattered dialysis, after 6.8h to salt rejection rate be 65% when, it is out of service.
A desalination silk fibroin protein solution is taken, adds 2000ml deionized waters to carry out the secondary desalination of electrodialysis in water tank, adjusted
It is 40L/h to save silk fibroin protein solution flow, and the flow of water is 20L/h, is passed through pole water, and the flow for adjusting pole water is 3L/h, is circulated
After waterflow stabilization, connection dc source, control electric current 0.1A, when silk fibroin protein solution electrical conductivity reaches 200 μ S/cm, (i.e. TDS is
0.1g/L) stop desalination during left and right, measure the desalination time for 7h.Final salt rejection rate is 99.98%, and the fibroin albumen rate of recovery is
91.0%, power consumption is less than 0.0175KWh.
Embodiment 7
Take 120g silk fibroin protein solutions in material box, add the deionized water of 100ml, concentration dilution to 4%, go from
2000ml deionized waters are added in sub- water tank, it is 40L/h to control silk fibroin protein solution flow, and the flow of water is 20L/h, is expanded
Desalination of scattered dialysis, after 6.8h to salt rejection rate be 65% when, it is out of service.
A desalination silk fibroin protein solution is taken, adds 2000ml deionized waters to carry out the secondary desalination of electrodialysis in water tank, adjusted
It is 40L/h to save silk fibroin protein solution flow, and the flow of water is 20L/h, is passed through pole water, and the flow for adjusting pole water is 3L/h, is circulated
After waterflow stabilization, connection dc source, control electric current 0.3A, when silk fibroin protein solution electrical conductivity reaches 200 μ S/cm, (i.e. TDS is
0.1g/L) stop desalination during left and right, measure the desalination time for 3.2h.Final salt rejection rate is 99.98%, and the fibroin albumen rate of recovery is
91.3%, power consumption is less than 0.024KWh.
Comparative example 1
Take 120g silk fibroin protein solutions in material box, add the deionized water of 100ml, concentration dilution to 4%, go from
2000ml deionized waters are added in sub- water tank, it is 40L/h to control silk fibroin protein solution flow, and the flow of water is 20L/h, is expanded
Desalination of scattered dialysis, after 5.2h to salt rejection rate be 40% when, it is out of service.
A desalination silk fibroin protein solution is taken, adds 2000ml deionized waters to carry out the secondary desalination of electrodialysis in water tank, adjusted
It is 40L/h to save silk fibroin protein solution flow, and the flow of water is 20L/h, is passed through pole water, and the flow for adjusting pole water is 3L/h, is circulated
After waterflow stabilization, connection dc source, control electric current 0.2A, when silk fibroin protein solution electrical conductivity reaches 200 μ S/cm, (i.e. TDS is
0.1g/L) stop desalination during left and right, measure the desalination time for 5.7h.Final salt rejection rate is 99.96%, and the fibroin albumen rate of recovery is
94.04%, power consumption is 0.071KWh.
Comparative example 2
Take 120g silk fibroin protein solutions in material box, add the deionized water of 100ml, concentration dilution to 4%, go from
2000ml deionized waters are added in sub- water tank, it is 40L/h to control silk fibroin protein solution flow, and the flow of water is 20L/h, is expanded
Desalination of scattered dialysis, after 26h to salt rejection rate be 90% when, it is out of service.
A desalination silk fibroin protein solution is taken, adds 2000ml deionized waters to carry out the secondary desalination of electrodialysis in water tank, adjusted
It is 40L/h to save silk fibroin protein solution flow, and the flow of water is 20L/h, is passed through pole water, and the flow for adjusting pole water is 3L/h, is circulated
After waterflow stabilization, connection dc source, control electric current 0.2A, when silk fibroin protein solution electrical conductivity reaches 200 μ S/cm, (i.e. TDS is
0.1g/L) stop desalination during left and right, measure the desalination time for 1h.Final salt rejection rate is 99.90%, and the fibroin albumen rate of recovery is
83.74%, power consumption is less than 0.005KWh.
Respectively on the basis of the desalination time of the embodiment of the present invention 1 and energy consumption (water consume and power consumption), by the present invention and other
The desalination time of method compares with energy consumption, as shown in table 1：
The desalting effect of the various desalination process of table 1 compares
| Desalination process | The desalination time | Salt rejection rate/% | Water consume | Desalination power consumption |
| This technique | 1 | 99.98 | 1 | 1 |
| Bag filter | 6.3 | 99.79 | 8.6 | 0 |
| Nanofiltration | 1.2 | 98 | 4 | 48 |
| Electrodialysis | 0.9 | 99.5 | 3.2 | 2.9 |
Table 1 shows, the deionized water in the present invention is recycled, and the electrodialysis advanced desalination time is shorter, and pole water disappears
Consumption is also reduced, therefore water consume is far smaller than other techniques.In addition, the technique compared to only use electrodialysis desalination for, desalination
Time is close, and salt rejection rate is higher, and sharpest edges are that power consumption is less.So, the technique is reaching the situation compared with equipment with high desalinization
Under, the desalination time is shortened, reduce energy consumption.
The design parameter of other embodiments and comparative example is shown in Table 2, and unlisted parameter is same as Example 1.
Parameter in the other embodiments desalination processes of table 2
The above is only the preferred embodiment of the present invention, it is noted that for the common skill of the art
For art personnel, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications
Also should be regarded as present disclosure.
Claims (10)
1. a kind of desalination system of soluble silk fibroin protein solution, it is characterised in that including material box, diffusion dialysis module and electricity
Dialysis module, material box has two imports of the import of diffusion dialysis liquid and electrodialysis material inlet, and material outlet and electrodialysis original
Two outlets of material outlet, wherein, the diffusion dialysis liquid import of material box and material outlet are connected with diffusion dialysis module, material box
Electrodialysis material inlet and electrodialysis material outlet be connected with electrodialysis module.
2. desalination system according to claim 1, it is characterised in that the diffusion dialysis module include diffusion dialysis material pump,
Diffusion water pump, diffusion dialysis device and deionization water tank；Diffusion dialysis device is connected by diffusion dialysis material pump with material box, deionization
Water tank is connected by diffusion water pump with diffusion dialysis device.
3. desalination system according to claim 2, it is characterised in that the diffusion dialysis device is provided with material inlet, diffusion and oozes
Analysis liquid outlet, diffusion water inlet and diffusion water out；Material inlet and the outlet of diffusion dialysis liquid go out respectively with the raw material of material box
Mouth is connected with diffusion dialysis liquid import；Diffusion water inlet and spread water out respectively with the water out and water inlet of deionization water tank
It is connected；Preferably, the position of material inlet and the outlet of diffusion dialysis liquid takes diagonal to arrange in the diffusion dialysis device；Diffusion
Also diagonal is taken to arrange in the position of water inlet and diffusion water out.
4. the desalination system according to Claims 2 or 3, it is characterised in that the pipe between the material box and diffusion dialysis device
Material flow meter and feed pressure table are additionally provided with road；It is additionally provided with pipeline between the deionization water tank and diffusion dialysis device
Divergent flow gauge and diffusion water pressure table.
5. according to the arbitrary desalination system of claim 1-4, it is characterised in that the electrodialysis module includes electric osmose analysis of material
Pump, electrodialysis water pump, electric dialyzator and water tank；Electric dialyzator is connected by electric osmose analysis of material pump with material box, and water tank passes through electric osmose
Bleed pump is connected with electric dialyzator.
6. desalination system according to claim 5, it is characterised in that the electric dialyzator includes longitudinal alternating parallel arrangement
Enriched chamber and diluting compartment, the electrodialysis material inlet of the material box is connected with diluting compartment outlet；The electrodialysis raw material of material box
Outlet is connected with enriched chamber's import；Diluting compartment import and enriched chamber outlet respectively with the water outlet and concentrated water import phase of water tank
Even.
7. the desalination system according to claim 5 or 6, it is characterised in that the pipeline between the material box and electric dialyzator
On be additionally provided with a desalting soln flowmeter and a desalting soln pressure gauge；On pipeline between the water tank and electric dialyzator
It is additionally provided with electrodialytic water flowmeter and electrodialytic water pressure gauge.
8. a kind of desalination process of soluble silk fibroin protein solution, it is characterised in that usage right requires the arbitrary desalinations of 1-7
System, by silk fibroin protein solution by being passed through in material box in diffusion dialysis module, is diffused dialysis, obtains a desalination fibroin
Protein solution；A desalination silk fibroin protein solution is passed through in the material box of electrodialysis module again carry out electrodialysis, obtains secondary
The silk fibroin protein solution that desalination silk fibroin protein solution, i.e. desalination are completed.
9. desalination process according to claim 8, it is characterised in that comprise the following steps：
(1), a desalination is carried out using diffusion dialysis：Open diffusion dialysis mould fast, close electrodialysis module, the silk in material box
(silk fibroin protein solution is by silk through Na for fibroin solution2CO3Degumming, calcium chloride-ethanol-water Ternary System dissolving is obtained) it is logical
Cross diffusion dialysis material pump to enter from the material inlet of diffusion dialysis device according to liquid linear velocity 1-5cm/s, after diffusion dialysis
Export out from diffusion dialysis liquid, circulation is flowed back in material box, diffusion water pump is by the deionized water in deionization water tank with linear speed
Degree 1-5cm/s flows out from diffusion water inlet suction diffusion dialysis device from diffusion water out, and recycle stream is gone back in ionized water tank；
When the salt content of deionized water in deionization water tank is 60-70% (preferably 65%) of initial salt content, stop diffusion dialysis,
Obtain a desalination silk fibroin protein solution；The linear velocity ratio of silk fibroin protein solution and deionized water is (1-2)：1, (preferably 2：1)；
(2), secondary desalination is carried out using electrodialysis：Close diffusion dialysis mould fast, open electrodialysis module, switch on power (electric current
Less than 0.3A, preferred 0.2A), electric osmose analysis of material pump is with liquid linear velocity 1-5cm/s by a desalination fibroin egg in material box
The diluting compartment of white solution Jing electrodialysis liquid import suction electric dialyzators, Jing after electrodialysis desalination, from the electrodialysed product of diluting compartment
Outlet is flowed out, and circulation is flowed in material box, while by the deionized water in water tank with liquid linear velocity 1-5cm/s from electric dialyzator
Water outlet enter enriched chamber, carry out after ion exchange with a desalination silk fibroin protein solution, from enriched chamber outlet flow out, follow
Circulation enters in water tank；When the electrical conductivity of silk fibroin protein solution in material box is below 200 μ S/cm, stop electrodialysis, obtain two
Secondary desalination silk fibroin protein solution, i.e., the silk fibroin protein solution that desalination is completed is derived by electrodialysed product outlet；
Preferably, dividing plate of the concentration of silk fibroin protein solution in below 6wt%, diffusion dialysis device before diffusion dialysis in material box
Thickness is 2mm-3mm, and the block board thickness of diluting compartment is 2mm-3mm in electric dialyzator, and the block board thickness of enriched chamber is 0.5mm；It is excellent
Choosing, it by anion exchange resin and cationic ion-exchange resin mass ratio is 1 that the ion exchange resin filled in diluting compartment is:1-
1:1.5 hybrid resins for obtaining.
10. a kind of production method of soluble fibroin albumen, it is characterised in that take silk Na2CO3Degumming, calcium chloride-ethanol-
Water ternary system dissolving obtains silk fibroin protein solution, then desalination process is carried out to silk fibroin protein solution described in Jing claims 8 or 9
Desalination, obtains secondary desalination silk fibroin protein solution, finally carries out freeze-drying, that is, obtain fibroin albumen.
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| CN113023844A (en) * | 2019-12-09 | 2021-06-25 | 中国科学院过程工程研究所 | Method for treating salt-containing fermentation waste liquid by combining diffusion dialysis with electrodialysis |
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