CN108311090A - A kind of spraying crosslinking apparatus preparing calcium alginate electric actuation film and cross-linking method of spraying - Google Patents
A kind of spraying crosslinking apparatus preparing calcium alginate electric actuation film and cross-linking method of spraying Download PDFInfo
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- CN108311090A CN108311090A CN201810231298.5A CN201810231298A CN108311090A CN 108311090 A CN108311090 A CN 108311090A CN 201810231298 A CN201810231298 A CN 201810231298A CN 108311090 A CN108311090 A CN 108311090A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/26—Nozzle-type reactors, i.e. the distribution of the initial reactants within the reactor is effected by their introduction or injection through nozzles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D19/00—Degasification of liquids
- B01D19/0073—Degasification of liquids by a method not covered by groups B01D19/0005 - B01D19/0042
- B01D19/0078—Degasification of liquids by a method not covered by groups B01D19/0005 - B01D19/0042 by vibration
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/006—Heteroglycans, i.e. polysaccharides having more than one sugar residue in the main chain in either alternating or less regular sequence; Gellans; Succinoglycans; Arabinogalactans; Tragacanth or gum tragacanth or traganth from Astragalus; Gum Karaya from Sterculia urens; Gum Ghatti from Anogeissus latifolia; Derivatives thereof
- C08B37/0084—Guluromannuronans, e.g. alginic acid, i.e. D-mannuronic acid and D-guluronic acid units linked with alternating alpha- and beta-1,4-glycosidic bonds; Derivatives thereof, e.g. alginates
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Abstract
The present invention provides a kind of spraying crosslinking apparatus preparing calcium alginate electric actuation film and cross-linking method of spraying, spraying cross-linking method is by sodium alginate and calcium chloride solution according to best crosslinking concentration proportioning, and plasticizer glycerine is added dropwise, when being atomized crosslinking, constant temperature stirs in crosslinking apparatus of spraying.Main process steps include:Spraying cross-linking reaction, ultrasonic vibration deaeration and vacuum constant temperature drying.The key structural feature of spraying crosslinking apparatus:Square rack pedestal, size is identical as magnetic stir plate, plays stable support function;Ring grille mounting for fixing cross-linking reaction container (500ml beakers), and can monitor all spraying cross-linking process by vacancy between grid;Spraying port lid be provided with two identical size through-holes, with realize air pump spray gun extend into crosslinking container in and stability.The spraying cross-linking method of the present invention is used with matched with devices, and conventional efficient can not only be substantially improved, but also can be effectively improved the tensile strength and actuating stability of calcium alginate electric actuation film.
Description
Technical field
The present invention relates to a kind of spraying crosslinking apparatus preparing calcium alginate electric actuation film and spraying cross-linking methods.
Background technology
With the continuous development of bionic engineering and intellectual material, bionics artificial thews come into being, and apply it to machine
The fields such as device people, wearable sensors and MEMS can simplify mechanical structure, improve energy conversion efficiency.Alginic acid
Sodium is extracted from seaweed, is not advised by α-Isosorbide-5-Nitrae-L- guluronic acids chain link (G) and β-Isosorbide-5-Nitrae-D-MANNOSE aldehydic acid chain link (M)
A kind of linear, the nontoxic natural polymers being then formed by connecting, with cheap, hydrophily is strong, biocompatibility
The advantages that good and biodegradable.When itself and Ca2+When contact, interannular oxygen, hydroxyl oxygen and the carboxyl in GG structural units can be passed through
Oxygen and Ca2+It is coordinated and transient gel, the calcium alginate hydrogel with " egg box " structure is formed, as biomimetic prosthetic
The research of the electric actuation film, artificial skin and biological medicine material of muscle, suffers from very extensive application prospect.Currently used for
The crosslinking process method for preparing calcium alginate hydrogel mainly has hydrodynamic force spin processes and swelling infusion process.However, these methods
It can only realize surface and the shallow-layer crosslinking of gel, and can not go deep into inside it.The crosslinking of thus obtained calcium alginate hydrogel
Degree is relatively low and ectonexine is uneven, thus its to be dried to the poor controllability after electric actuation film, tensile strength smaller, can not be for imitative
Raw artificial-muscle Reusability.Therefore, research and probe one kind is easy to operate, effective crosslinking process method and crosslinking dress
It sets, there is important value.
《Textile science is studied》Periodical, 2014 Published in China Pharmacy《The preparation and application of calcium alginate hydrogel fiber》In article
Use a kind of crosslinking process method of hydrodynamic force spinning, using certain density sodium alginate soln, according to certain speed from
In the concordant syringe needle point in end, it is injected into coagulating bath (calcium chloride solution), it is fine to form solid-state calcium alginate hydrogel
Dimension.But the cross-linking reaction is almost to be completed in sodium alginate jet surface moment and can not penetrate into inside it, and it is difficult to control
The plastic shape of hydrogel processed.Meanwhile can be accumulated as cross-linked network structure based on the calcium alginate G groups under the method, and
Cause the internal structure of electric actuation film it is mixed and disorderly it is unordered, there is stress concentration, then seriously affect its and activate performance.
Invention content
The purpose of the invention is to provide a kind of significant effect, the environmentally protective spray for preparing calcium alginate electric actuation film
Mist cross-linking method, that is, cross-linking method of spraying;Its definite principle is suitble to commonly used;Also provide kind of a simple and effective, low-cost
The crosslinking apparatus for preparing calcium alginate electric actuation film, that is, crosslinking apparatus of spraying;Its is simple in structure, easily operated, and it is more to meet repetition
Secondary use.When the two matches, the best crosslinking of sodium alginate soln and calcium chloride solution matches, and reality can both be substantially improved
Efficiency is tested, and the tensile strength and actuating stability of calcium alginate electric actuation film can be effectively improved.
The object of the present invention is achieved like this:A kind of spraying crosslinking apparatus preparing calcium alginate electric actuation film, including
Bracket base, is located at ring grid at the ring grille mounting for fixing spraying cross-linking reaction container being uniformly arranged on bracket base
Spraying port lid above lattice holder, the bracket base are square structure, and spray holes cap surface opens that there are two size is identical
Through-hole.
A kind of spraying cross-linking method preparing calcium alginate electric actuation film, including the spraying crosslinking apparatus, step is such as
Under:
Step 1:Prepare sodium alginate soln and calcium chloride solution:
It weighs 1.25g sodium alginates to be dissolved in 50ml distilled water, is placed in 50 DEG C of heating stirrings of water-bath on magnetic stirring apparatus
20min waits for that solution is completely dissolved, and 2ml glycerine is added dropwise, and continues constant temperature stirring 10min and causes to be uniformly mixed;Meanwhile quickly measuring nothing
Water calcium chloride granules 0.105g prepares a concentration of 1.05mg/ml calcium chloride solutions 100ml;
Step 2:Carry out spraying cross-linking reaction:
By the complete cover buckle of square rack pedestal for crosslinking apparatus of spraying on the platform of magnetic stirring apparatus, then spraying friendship
Connection reaction vessel is put into ring grille mounting;Prepared sodium alginate soln and calcium chloride solution are drawn into two respectively
In air pump spray gun, and by two identical size through-holes on spray holes cap surface, it is respectively protruding into cross-linking reaction container and protects
It is fixed to keep steady;Then, at the same be atomized ejection carry out continue cross-linking reaction, crosslinking gained calcium alginate hydrogel solution, stirred by magnetic force
It mixes reaction vessel on device to collect, and remains 50 DEG C of constant temperature stirrings, until 15min after reaction;
Step 3:Complete ultrasonic vibration deaeration:
The sink temperature of pre-set ultrasonic oscillator is 50 DEG C, after temperature reaches, is put into and fills calcium alginate
The beaker of hydrogel solution, and ultrasonic oscillation frequency 20KHz is set, concussion inclined heated plate 20min;
Step 4:Carry out vacuum constant temperature drying:
The calcium alginate hydrogel solution uniform and stable handled through ultrasonic vibration deaeration is cast and pours into homemade glass
It in mold, is placed in vacuum drying chamber, and the arrange parameter of vacuum drying chamber is:Temperature 60 C, vacuum degree -0.085MPa,
Freeze-day with constant temperature time 18h.Period opens drying box door 15min, the saturated steam in case is discharged, then again every 3h
Vacuumize freeze-day with constant temperature;
Step 5:Realization standard cuts molding:
After the calcium alginate hydrogel solution in vacuum drying chamber is completely dried film forming, taking-up carries out cutting molding.
Compared with prior art, the beneficial effects of the invention are as follows:The present invention is directed to the friendship for preparing calcium alginate electric actuation film
Join process, using spraying cross-linking method, i.e., by sodium alginate soln and calcium chloride solution, be atomized and spray in crosslinking apparatus,
Realization be sufficiently mixed, the new crosslinking process method of homogeneous cross-link.Two kinds of solution are heated and be atomized mixing respectively, can be increased
Contact surface area when it being added to crosslink reaction, thus the crosslinking concentration proportioning of the two can be greatly improved, so that alginic acid
The mechanical strength and flexibility of calcium hydrogel get a promotion.Meanwhile the ectonexine network structure of hydrogel also achieves abundant friendship
Connection, makes it dry that the inner homogeneous after film forming is consistent, electric actuation performance is stably and controllable, service life extends.
The experiment crosslinking apparatus of the cooperation spraying crosslinking process method of the present invention, that is, crosslinking apparatus of spraying, using ring grid
The mode that lattice holder is combined with each other with spraying port lid, overall structure are simple, easily operated, of low cost.Making material simultaneously
Environmentally protective, free from extraneous odour itself is suitble to repeated multiple times use, is easy to clean.It, can be most based on the spraying crosslinking apparatus of the present invention
Reduce human factor to limits, to the de-stabilising effect of cross-linking reaction process, to ensure calcium alginate made from every batch of
The electromechanical properties of electric actuation film, stable and consistent.
Description of the drawings
Fig. 1 is spraying crosslinking process flow chart;
Fig. 2 is the whole schematic three dimensional views of spraying crosslinking apparatus;
Fig. 3 is bracket base and ring lattice structure figure;
Fig. 4 is the structural schematic diagram of spraying port lid.
Specific implementation mode
Present invention is further described in detail with specific implementation mode below in conjunction with the accompanying drawings.
The present invention provides a kind of spraying crosslinking process method preparing calcium alginate electric actuation film, is by sodium alginate soln
It is matched according to a certain concentration with calcium chloride solution, when spraying crosslinking, constant temperature stirs in crosslinking apparatus of spraying.Then, it is added dropwise and increases
Modeling agent glycerine is put into supersonic wave cleaning machine after solution stirs evenly and shakes deaeration.Finally, it is placed in vacuum drying chamber, into
Row vacuum constant temperature is dried, so that calcium alginate electric actuation film drying and moulding.Therefore, Main process steps include:Spraying crosslinking
Reaction, ultrasonic vibration deaeration and vacuum constant temperature dry three processes.
(1) spraying cross-linking reaction:It weighs 1.25g sodium alginates to be dissolved in 50ml distilled water (i.e. 25mg/ml), 50 DEG C of water-bath
2ml glycerine is added dropwise in heating stirring 20min, continues constant temperature stirring 10min and causes to be uniformly mixed.Prepare a concentration of 1.05mg/ml chlorinations
Calcium solution 100ml.Then, sodium alginate soln and calcium chloride solution are sucked respectively in air pump spray gun, and in spraying crosslinking dress
In setting, while being atomized ejection and carrying out continuing cross-linking reaction.Gained calcium alginate solution is received by 500ml beakers on magnetic stirring apparatus
Collection, and 50 DEG C of constant temperature stir 15min.
(2) ultrasonic vibration deaeration:The beaker of calcium alginate hydrogel solution will be filled, is placed in the sink of ultrasonic oscillator
In, it carries out ultrasonic vibration deaeration and handles 20min, 50 DEG C of set temperature, concussion frequency 20KHz.With lasting ultrasonic oscillation,
The minute bubbles disperseed everywhere in solution can gradually float and be gathered in solution surface to break apart, will then contain residual gas
The surface solution of bubble removes.
(3) vacuum constant temperature is dried:By calcium alginate hydrogel solution, uniform and stable it is cast and pours into homemade glass mold
In, it is placed in vacuum drying chamber, arrange parameter:Temperature 60 C, vacuum degree -0.085MPa, freeze-day with constant temperature time 18h.Period,
Drying box door 15min, which is opened, every 3h then vacuumizes freeze-day with constant temperature again so that saturated steam in case is discharged.Wait for that solution is complete
White drying forms a film, and takes out and cuts molding.
In above steps, sodium alginate powder (90%), glycerine (glycerine) and anhydrous calcium chloride particle are analysis
Pure (Analytical Reagent, AR) drug.
A kind of spraying crosslinking apparatus preparing calcium alginate electric actuation film, main includes some such structure features:
(1) bracket base of crosslinking apparatus is square, the platform size phase of size and experiment magnetic stirring apparatus used
Together, to reach whole covering, to play stable support function;
(2) ring grille mounting is designed, for fixed spraying cross-linking reaction container (500ml beakers), and grid can be passed through
Between vacancy, observe all spraying cross-linking process, to monitor its extent of reaction and progress in real time;
(3) spray holes cap surface is opened there are two the identical through-hole of size, to keep the stability of air pump Spray gun nozzle, while again
It can extend into crosslinking container chamber, meet requirement of experiment.
As shown in Figure 1, a kind of spraying crosslinking process flow chart preparing calcium alginate electric actuation film of the present invention, main to walk
Suddenly include:Preparation sodium alginate soln, preparation calcium chloride solution, spraying cross-linking reaction, ultrasonic vibration deaeration, vacuum constant temperature are dry
Dry, standard cuts six processes such as molding.Meanwhile a kind of spraying crosslinking apparatus preparing calcium alginate electric actuation film, such as Fig. 2 institutes
Show, is mainly made of main body rack and spraying port lid two parts.Its CONSTRUCTED SPECIFICATION feature includes:With magnetic stirring apparatus used in experiment
The identical square rack pedestal of platform size, for fixed spraying cross-linking reaction container (500ml beakers) and real time monitoring
The ring grille mounting of cross-linking reaction degree, and realize the spray holes of air pump rifle mouth application and two identical sizes of stability
Cap surface through-hole.
First, sodium alginate soln and calcium chloride solution are prepared.Prepare to analyze pure (AR) drug:Sodium alginate powder
(90%), glycerine (glycerine) and anhydrous calcium chloride particle.1.25g sodium alginates, which are weighed, using assay balance is dissolved in 50ml distillations
In water (i.e. 25mg/ml), it is placed in 50 DEG C of heating stirring 20min of water-bath on magnetic stirring apparatus.Wherein, the mixing speed of magneton is rotated
Unsuitable too fast or excessively slow, generating small vortex with the solution surface in beaker is advisable, and avoids sodium alginate soln from generating a large amount of small
Bubble.It waits for that solution is completely dissolved, 2ml glycerine is added dropwise, continue constant temperature stirring 10min and cause to be uniformly mixed, made with playing moisturizing plasticising
With.Meanwhile anhydrous calcium chloride particle 0.105g is quickly measured, prepare a concentration of 1.05mg/ml calcium chloride solutions 100ml.
Secondly, spraying cross-linking reaction is carried out.It is in conjunction with Fig. 3 and Fig. 4, the square rack pedestal 1 for crosslinking apparatus of spraying is complete
Full cover buckle plays stable support function on the platform of magnetic stirring apparatus;Cross-linking reaction container (500ml beakers) is put into ring again
In grille mounting 2, to realize fixation.At this point, prepared sodium alginate soln and calcium chloride solution are drawn into two respectively
In branch air pump spray gun, and by two identical size through-holes 3 on spray holes cap surface, be respectively protruding into cross-linking reaction container and
It keeps stablizing.Then, it while being atomized ejection and carries out continuing cross-linking reaction, spray velocity can lead to by air pump pressure controlling
Cross vacancy between ring grid, real-time observing response degree.In addition, crosslinking gained calcium alginate hydrogel solution, by magnetic stirring apparatus
Upper reaction vessel (500ml beakers) is collected, and remains 50 DEG C of constant temperature stirrings, until 15min after reaction.
Again, ultrasonic vibration deaeration is completed.The sink temperature of pre-set ultrasonic oscillator (equipped 2000W voltage-stablizers)
Degree is 50 DEG C, after temperature reaches, is put into the beaker for filling calcium alginate hydrogel solution.At this point, setting ultrasonic oscillation frequency
Rate 20KHz, concussion inclined heated plate 20min.With lasting ultrasonic oscillation, the minute bubbles disperseed everywhere in solution can be gradual
It floats and is gathered in solution surface to break apart, then remove the surface solution containing residual bubbles.
Then, vacuum constant temperature drying is carried out.The calcium alginate hydrogel solution that will be handled through deaeration, is cast to uniform and stable
It pours into homemade glass mold, is placed in the vacuum drying chamber being previously set, arrange parameter:Temperature 60 C, vacuum degree-
0.085MPa, freeze-day with constant temperature time 18h.Period opens drying box door 15min every 3h, the saturated steam in case is discharged,
Then freeze-day with constant temperature is vacuumized again.Vacuum degree is set herein so that forms negative pressure in drying box, remains in sea with thorough discharge
Minute bubbles in alginic acid calcium solution, and then ensure that the inner homogeneous after its drying and forming-film is consistent, surface is smooth and actuating property
It can stablize.
Finally, realize that standard cuts molding.It waits in vacuum drying chamber, calcium alginate hydrogel solution is completely dried film forming
Afterwards, it takes out and carries out cutting molding, to obtain the calcium alginate electric actuation film of uniform specification, function admirable.
To sum up, the present invention relates to a kind of spraying crosslinking process method preparing calcium alginate electric actuation film and spraying crosslinking dresses
It sets.Spraying cross-linking method is sodium alginate and calcium chloride solution to be crosslinked concentration proportioning according to best, and plasticizer glycerine is added dropwise,
When being atomized crosslinking, constant temperature stirs in spraying crosslinking apparatus.Main process steps include:Spraying cross-linking reaction, ultrasonic vibration deaeration
It is dried with vacuum constant temperature.The key structural feature of spraying crosslinking apparatus:Square rack pedestal, size are flat with magnetic stirring apparatus
Platform is identical, plays stable support function;Ring grille mounting for fixing cross-linking reaction container (500ml beakers), and can pass through grid
Compartment vacancy monitors all spraying cross-linking process;Spraying port lid is provided with two identical size through-holes, to realize that air pump spray gun stretches into
To crosslinking container in and stability.The spraying cross-linking method of the present invention is used with matched with devices, and conventional efficient can both be substantially improved,
It can be effectively improved the tensile strength and actuating stability of calcium alginate electric actuation film again.
Claims (2)
1. a kind of spraying crosslinking apparatus preparing calcium alginate electric actuation film, it is characterised in that:Including bracket base, it is uniformly arranged
The ring grille mounting for fixed spraying cross-linking reaction container on bracket base, the spray holes above ring grille mounting
Lid, the bracket base are square structure, and spray holes cap surface opens that there are two the identical through-holes of size.
2. a kind of spraying cross-linking method preparing calcium alginate electric actuation film, it is characterised in that:Including spray described in claim 1
Mist crosslinking apparatus, steps are as follows:
Step 1:Prepare sodium alginate soln and calcium chloride solution:
It weighs 1.25g sodium alginates to be dissolved in 50ml distilled water, is placed in 50 DEG C of heating stirring 20min of water-bath on magnetic stirring apparatus,
It waits for that solution is completely dissolved, 2ml glycerine is added dropwise, continue constant temperature stirring 10min and cause to be uniformly mixed;Meanwhile quickly measuring anhydrous chlorination
Calcium particle 0.105g prepares a concentration of 1.05mg/ml calcium chloride solutions 100ml;
Step 2:Carry out spraying cross-linking reaction:
By the complete cover buckle of square rack pedestal for crosslinking apparatus of spraying on the platform of magnetic stirring apparatus, then spraying crosslinking is anti-
Container is answered to be put into ring grille mounting;Prepared sodium alginate soln and calcium chloride solution are drawn into two air pumps respectively
In spray gun, and by two identical size through-holes on spray holes cap surface, it is respectively protruding into cross-linking reaction container and keeps steady
It is fixed;Then, at the same be atomized ejection carry out continue cross-linking reaction, crosslinking gained calcium alginate hydrogel solution, by magnetic stirring apparatus
Upper reaction vessel is collected, and remains 50 DEG C of constant temperature stirrings, until 15min after reaction;
Step 3:Complete ultrasonic vibration deaeration:
The sink temperature of pre-set ultrasonic oscillator is 50 DEG C, after temperature reaches, is put into and fills calcium alginate water-setting
The beaker of sol solution, and ultrasonic oscillation frequency 20KHz is set, concussion inclined heated plate 20min;
Step 4:Carry out vacuum constant temperature drying:
The calcium alginate hydrogel solution uniform and stable handled through ultrasonic vibration deaeration is cast and pours into homemade glass mold
In, it is placed in vacuum drying chamber, and the arrange parameter of vacuum drying chamber is:Temperature 60 C, vacuum degree -0.085MPa, constant temperature
Drying time 18h.Period opens drying box door 15min every 3h, the saturated steam in case is discharged, then takes out again true
Empty freeze-day with constant temperature;
Step 5:Realization standard cuts molding:
After the calcium alginate hydrogel solution in vacuum drying chamber is completely dried film forming, taking-up carries out cutting molding.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110013348A (en) * | 2019-04-09 | 2019-07-16 | 河南理工大学 | For the anti-preparation facilities and method for sticking artificial blood vessel's material |
CN111701078A (en) * | 2020-04-20 | 2020-09-25 | 上海以心医疗器械有限公司 | Method for improving cross-linking degree of biological tissue |
CN114425302A (en) * | 2022-01-19 | 2022-05-03 | 西安交通大学 | Activated carbon gel particles with high specific surface area, and spray preparation method, application and preparation device thereof |
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CN107619487A (en) * | 2017-10-11 | 2018-01-23 | 哈尔滨工程大学 | A kind of preparation method of the calcium cross-linked sodium alginate electric drive film of chlorination |
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CN204564180U (en) * | 2015-03-20 | 2015-08-19 | 杭州职业技术学院 | A kind of glass apparatus rack for cylindrical constant temperature water bath |
CN105328905A (en) * | 2015-11-09 | 2016-02-17 | 西安交通大学 | 3D printing system and technology of coaxial sprayer and enhanced type hollow gel pipe of coaxial sprayer |
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CN110013348A (en) * | 2019-04-09 | 2019-07-16 | 河南理工大学 | For the anti-preparation facilities and method for sticking artificial blood vessel's material |
CN111701078A (en) * | 2020-04-20 | 2020-09-25 | 上海以心医疗器械有限公司 | Method for improving cross-linking degree of biological tissue |
CN114425302A (en) * | 2022-01-19 | 2022-05-03 | 西安交通大学 | Activated carbon gel particles with high specific surface area, and spray preparation method, application and preparation device thereof |
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