CN107619487A - A kind of preparation method of the calcium cross-linked sodium alginate electric drive film of chlorination - Google Patents
A kind of preparation method of the calcium cross-linked sodium alginate electric drive film of chlorination Download PDFInfo
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- CN107619487A CN107619487A CN201710939618.8A CN201710939618A CN107619487A CN 107619487 A CN107619487 A CN 107619487A CN 201710939618 A CN201710939618 A CN 201710939618A CN 107619487 A CN107619487 A CN 107619487A
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Abstract
The present invention provides a kind of preparation method of the calcium cross-linked sodium alginate electric drive film of chlorination, glycerine is added as dressing agent after carrying out cross-linking reaction according to certain mol proportion using sodium alginate and calcium chloride, the solution of generation disposable generation calcium cross-linked sodium alginate electric drive film of chlorination after ultrasonic wave deaeration and vacuum drying treatment, including three liquid phase cross-linking reaction, ultrasonic wave deaeration processing and high temperature drying steps.The present invention is green, and cost is cheap, and step is simple, is adapted to large-scale production, caused sodium alginate electric drive film, in the alternative conventional ADS driving structure in flexible mechanical field, has good tensile strength and pliability.
Description
Technical field
The present invention relates to the preparation method of sodium alginate electric drive film, more particularly to a kind of calcium cross-linked sodium alginate of chlorination
The preparation method of electric drive film.
Background technology
The one kind of gelatin polymer quasi-driver as ion drives, the advantages such as preparation technology simple low with its cost,
Studied a question as currently hotter.Currently, in gel polymerisation species electric drive the material of drive membrane mainly using IPMC with
Chitosan, but IPMC output stabilities are poor, the life-span is low, chitosan molecule amount is low, dissolubility is bad, causes current gel polymerisation
Limitation is compared in the application of thing electric drive film.Sodium alginate is the macromolecule polysaccharide extracted from brown alga plant, has good peace
Full property and recyclability, the sodium alginate soln prepared have good film forming, and institute's film-forming flexibility is good and transparency is high.
As crosslinking agent with sodium alginate chelation can occur for calcium chloride, the strand of sodium alginate is combined even closer, collaboration
Act on stronger, the interaction of chain interchain ultimately results in the formation of three dimensional network structure, i.e. gel state, improves electric drive film
Tensile strength, thickness and pliability, so as to drastically increase the combination property of drive membrane.The preparation method of the present invention uses
Sodium alginate adds glycerine as dressing agent after carrying out cross-linking reaction according to certain mol proportion with calcium chloride, and the solution of generation is through super
Sound wave deaeration and the disposable generation calcium cross-linked sodium alginate electric drive film of chlorination after vacuum drying treatment, cost is cheap, system
Standby overall process is green, pollution-free, and traditional structure can be substituted in fields such as bionics, flexible mechanicals, avoids the dress of complexity
With process, there is important use value.
The content of the invention
The invention aims to provide a kind of preparation method of the calcium cross-linked sodium alginate electric drive film of chlorination, green
Environmental protection, cost is cheap, and step is simple, is adapted to large-scale production, caused sodium alginate electric drive film can in flexible mechanical field
Conventional ADS driving structure is substituted, there is good tensile strength and pliability.
The object of the present invention is achieved like this：Step is as follows：
Step 1：Liquid phase cross-linking reaction：
1.5g sodium alginates are put into be placed under water bath in 50mL distilled water and heated, are stirred using magnetic stirring apparatus
Mix, sodium alginate is completely dissolved in distilled water；0.085g anhydrous calcium chlorides are put into 100ml distilled water and are stirred；
Sodium alginate aqueous solution is added slowly in calcium chloride water along glass bar afterwards, sodium alginate is handed over calcium chloride
Connection reaction, instill 2ml glycerine after full cross-linked and continue heating stirring until glycerine fully dissolves；
Step 2：Ultrasonic wave deaeration is handled：
The beaker for filling calcium chloride crossslinked sodium alginate solution is put into supersonic wave cleaning machine, opens electrical equipment cabinet panel
" power control switch ", and rinse bath heating-up temperature is set as 40 DEG C~50 DEG C, rinse bath heater switch is opened, groove to be cleaned arrives
Up to after design temperature, ultrasonic power switch on electrical equipment cabinet panel is opened, power output is slowly adjusted, is shaken, at deaeration
Reason；
Step 3：High temperature drying：
Will shake, deaeration processing after mixed solution be uniformly cast in assembled square glass mould, be positioned over
4-6h is dried in vacuum drying chamber, drying temperature is arranged to 50 DEG C, vacuum zero, after obtaining sodium alginate and calcium chloride crosslinking
The drive membrane of formation.
Present invention additionally comprises some such architectural features：
1. the sodium alginate soln uniform stirring process in step 1 is specifically：Stirrer is added, starts magnetic stirring apparatus
Stirring, mixing speed is unsuitable too fast or excessively slow, and it is 50 DEG C to set whipping temp, and mixing time is set as 50min, makes sodium alginate
It is substantially dissolved in distilled water.
2. addition is 8%~10% as the concentration of the glycerine of dressing agent in step 1.
3. the 220V/50Hz power supplys that the supersonic generator power supply in step 2 is single use, and equipped more than 2000W
Voltage-stablizer, supersonic wave cleaning machine frequency setting are that 20KHz sonification powers are 200W~500W, ultrasonic time be 30min~
1h。
4. the drying 4-6h described in step 3 is specially：It is dried in vacuo every 1h, opens drying box 20min, is accelerated dry
Hydrone evaporates in dry case.
Compared with prior art, the beneficial effects of the invention are as follows：1st, the sodium alginate (sodium in the present invention
Alginate) it is the macromolecule polysaccharide that is extracted from brown alga plant, the faint yellow unsetting powder of odorless, tasteless is soluble in water,
Good security, biocompatibility, film forming and gelling performance make its be widely used in textile industry, medical industry and
The fields such as food industry, easily obtain and cost is cheap, therefore there is preferable economy and practicality.When sodium alginate and chlorine
After change calcium crosslinks reaction, calcium ion is located in egg carton as egg, is collectively forming " egg carton " structure with G blocks, makes sea
The strand of mosanom combines even closer, and synergy is stronger, improve the tensile strength of electric drive film, thickness with it is flexible
Property, so as to drastically increase its combination property.2nd, the present invention is a kind of system of the calcium cross-linked sodium alginate electric drive film of chlorination
Preparation Method, and in particular to three liquid phase cross-linking reaction, ultrasonic wave deaeration processing and vacuum drying parts.Experimental facilities is simple, anti-
Should disposably complete, it is easy to operate, preparation process is gentle slowly, do not occur acutely chemical reaction, it is easily controllable, green,
Free from extraneous odour.The design of preparation process is relatively reasonable, takes into full account that each side influence factor compensates, reduces because of operating process and people
For error caused by factor.3rd, because liquid phase cross-linking reaction method can be amplified according to production scale, so being adapted to batch production.
Brief description of the drawings
Fig. 1 is the flow chart of the present invention.
Embodiment
The present invention is described in further detail with embodiment below in conjunction with the accompanying drawings.
With reference to Fig. 1, a kind of preparation method of the calcium cross-linked sodium alginate electric drive film of chlorination of the invention, feature include with
Lower process：
Glycerine is added as dressing agent after carrying out cross-linking reaction according to certain mol proportion using sodium alginate and calcium chloride, it is raw
Into solution after ultrasonic wave deaeration and vacuum drying treatment the disposable generation calcium cross-linked sodium alginate electric drive film of chlorination,
Including three liquid phase cross-linking reaction, ultrasonic wave deaeration processing and high temperature drying steps.
(1) liquid phase cross-linking reaction：1.5g sodium alginates are put into be placed under water bath in 50mL distilled water and heated, are used
Magnetic stirring apparatus is stirred, and sodium alginate is completely dissolved in distilled water；0.085g anhydrous calcium chlorides are put into 100ml to steam
It is stirred in distilled water.Sodium alginate aqueous solution is added slowly in calcium chloride water along glass bar afterwards, makes alginic acid
Sodium carries out cross-linking reaction with calcium chloride, instills 2ml glycerine after full cross-linked and continues heating stirring until glycerine fully dissolves；
(2) ultrasonic wave deaeration is handled：The beaker for filling calcium chloride crossslinked sodium alginate solution is put into supersonic wave cleaning machine
In, electrical equipment cabinet panel " power control switch " is opened, and rinse bath heating-up temperature is set as 40 DEG C~50 DEG C, preferably 50 DEG C, open
Rinse bath heater switch is opened, after groove to be cleaned reaches design temperature, ultrasonic power switch on electrical equipment cabinet panel is opened, slowly adjusts
Whole power output, shaken, deaeration processing；
(3) high temperature drying：Mixed solution after concussion, deaeration processing is uniformly cast to assembled square glass mould
In, it is positioned in vacuum drying chamber and dries 4-6h, preferably 5h, drying temperature is arranged to 50 DEG C, vacuum zero, you can obtain
Sodium alginate and the drive membrane formed after calcium chloride crosslinking.
In the step (1), the processing method of sodium alginate soln uniform stirring process is to add stirrer, starts magnetic force
Agitator stirs, and mixing speed is unsuitable too fast or excessively slow, and it is 50 DEG C to set whipping temp, and mixing time is set as 50min, to burn
Water in the cup face, which produces small whirlpool, to be advisable, and sodium alginate is substantially dissolved in distilled water.
In the step (1), anhydrous calcium chloride water imbibition is extremely strong, after quality needed for must weighing as early as possible is taken out from reagent bottle
Pour into beaker and dissolve, and calcium chloride unnecessary during weighing must not be put back in reagent bottle again, in order to avoid pollution reagent.It is stirred
Cheng Wuxu is heated, and the time is set as that 10min can obtain calcium chloride solution.
In the step (1), addition dressing agent glycerol concentration is 8%~10%, preferably 8%.
In the step (2), 220V/50Hz power supplys, and equipped more than 2000W should be used alone in supersonic generator power supply
Voltage-stablizer, supersonic wave cleaning machine frequency setting are 20KHz, and sonification power is 200W~500W, preferably 300W, ultrasonic time
For 30min~1h, the preferably time is arranged to 40min.
In the step (3), it is dried in vacuo every 1h, drying box 20min need to be opened, is accelerated hydrone in drying box and steam
Hair, it is easy to keep vacuum in drying box, accelerates rate of drying.
To sum up, the present invention relates to a kind of preparation method of the calcium cross-linked sodium alginate electric drive film of chlorination.Especially with
Cheap sodium alginate and calcium chloride are raw material, and mixed solution is made by liquid phase cross-linking reaction method, then carry out ultrasonic wave and take off
Bubble handles high-temperature vacuum drying process again, obtains good mechanical properties and the splendid electric drive membrane preparation method of pliability.It is special
Sign is that the preparation method adds glycerine conduct after carrying out cross-linking reaction according to certain mol proportion with calcium chloride using sodium alginate
Dressing agent, the solution of generation is disposable after ultrasonic wave deaeration and vacuum drying treatment to generate the calcium cross-linked sodium alginate electricity of chlorination
Drive film, including three liquid phase cross-linking reaction, ultrasonic wave deaeration and high temperature drying steps.This method prepares overall process green ring
Protect, be pollution-free, effectively reducing the generation of bubble, using calcium chloride as crosslinking agent, chelating can occur with sodium alginate and make
With making the strand of sodium alginate, the stretching that can be effectively improved electric drive film is strong with reference to even closer, formation gel state
Degree, thickness and pliability, so as to drastically increase the combination property of drive membrane, it can be used to replace Traditional IP MC to drive with chitosan
Dynamic film, has important use value in fields such as bionics, flexible mechanicals.
Claims (9)
- A kind of 1. preparation method of the calcium cross-linked sodium alginate electric drive film of chlorination, it is characterised in that：Step is as follows：Step 1：Liquid phase cross-linking reaction：1.5g sodium alginates are put into be placed under water bath in 50mL distilled water and heated, are stirred using magnetic stirring apparatus, Sodium alginate is set to be completely dissolved in distilled water；0.085g anhydrous calcium chlorides are put into 100ml distilled water and are stirred；Afterwards Sodium alginate aqueous solution is added slowly in calcium chloride water along glass bar, makes sodium alginate with calcium chloride be crosslinked instead Should, instill 2ml glycerine after full cross-linked and continue heating stirring until glycerine fully dissolves；Step 2：Ultrasonic wave deaeration is handled：The beaker for filling calcium chloride crossslinked sodium alginate solution is put into supersonic wave cleaning machine, opens electrical equipment cabinet panel " power supply Controlling switch ", and rinse bath heating-up temperature is set as 40 DEG C~50 DEG C, rinse bath heater switch is opened, groove to be cleaned is reached and set After constant temperature degree, ultrasonic power switch on electrical equipment cabinet panel is opened, slowly adjusts power output, shaken, deaeration processing；Step 3：High temperature drying：Will shake, deaeration processing after mixed solution be uniformly cast in assembled square glass mould, be positioned over vacuum 4-6h is dried in drying box, drying temperature is arranged to 50 DEG C, vacuum zero, obtains being formed after sodium alginate is crosslinked with calcium chloride Drive membrane.
- 2. a kind of preparation method of the calcium cross-linked sodium alginate electric drive film of chlorination according to claim 1, its feature exist In：Sodium alginate soln uniform stirring process in step 1 is specifically：Stirrer is added, starts magnetic stirrer, stirs It is unsuitable too fast or excessively slow to mix speed, it is 50 DEG C to set whipping temp, and mixing time is set as 50min, makes sodium alginate fully molten Solution is in distilled water.
- 3. a kind of preparation method of the calcium cross-linked sodium alginate electric drive film of chlorination according to claim 1 or 2, its feature It is：Addition is 8%~10% as the concentration of the glycerine of dressing agent in step 1.
- 4. a kind of preparation method of the calcium cross-linked sodium alginate electric drive film of chlorination according to claim 1 or 2, its feature It is：The 220V/50Hz power supplys that supersonic generator power supply in step 2 is single use, and equipped more than 2000W voltage stabilizings Device, supersonic wave cleaning machine frequency setting are that 20KHz sonification powers are 200W~500W, and ultrasonic time is 30min~1h.
- 5. a kind of preparation method of the calcium cross-linked sodium alginate electric drive film of chlorination according to claim 3, its feature exist In：The 220V/50Hz power supplys that supersonic generator power supply in step 2 is single use, and equipped more than 2000W voltage-stablizers, Supersonic wave cleaning machine frequency setting is that 20KHz sonification powers are 200W~500W, and ultrasonic time is 30min~1h.
- 6. a kind of preparation method of the calcium cross-linked sodium alginate electric drive film of chlorination according to claim 1 or 2, its feature It is：Drying 4-6h described in step 3 is specially：It is dried in vacuo every 1h, opens drying box 20min, is accelerated in drying box Hydrone evaporates.
- 7. a kind of preparation method of the calcium cross-linked sodium alginate electric drive film of chlorination according to claim 3, its feature exist In：Drying 4-6h described in step 3 is specially：It is dried in vacuo every 1h, opens drying box 20min, accelerates water in drying box Molecule evaporates.
- 8. a kind of preparation method of the calcium cross-linked sodium alginate electric drive film of chlorination according to claim 4, its feature exist In：Drying 4-6h described in step 3 is specially：It is dried in vacuo every 1h, opens drying box 20min, accelerates water in drying box Molecule evaporates.
- 9. a kind of preparation method of the calcium cross-linked sodium alginate electric drive film of chlorination according to claim 5, its feature exist In：Drying 4-6h described in step 3 is specially：It is dried in vacuo every 1h, opens drying box 20min, accelerates water in drying box Molecule evaporates.
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| CN108410026A (en) * | 2018-03-20 | 2018-08-17 | 哈尔滨工程大学 | A kind of method that freeze-drying prepares calcium alginate Biological gel membrane |
| CN108484955A (en) * | 2018-03-20 | 2018-09-04 | 哈尔滨工程大学 | A kind of preparation method of calcium alginate electric actuation film using microwave vacuum low-temperature dry technology |
| CN110173919A (en) * | 2019-04-30 | 2019-08-27 | 东南大学 | The device of gas type ammonium hydroxide bromine heat pump performance is promoted based on electric drive membrane separation technique |
| CN113429602A (en) * | 2021-06-23 | 2021-09-24 | 哈尔滨工程大学 | Preparation process method of sodium alginate/carboxymethyl cellulose actuating membrane |
| CN113527732A (en) * | 2021-06-30 | 2021-10-22 | 哈尔滨工程大学 | Preparation method of polyvinyl alcohol-sodium alginate gel actuating membrane |
| CN113571345A (en) * | 2021-06-30 | 2021-10-29 | 哈尔滨工程大学 | Preparation process method of manganese dioxide doped graphene oxide electrode film |
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| CN108311090A (en) * | 2018-03-20 | 2018-07-24 | 哈尔滨工程大学 | A kind of spraying crosslinking apparatus preparing calcium alginate electric actuation film and cross-linking method of spraying |
| CN108410026A (en) * | 2018-03-20 | 2018-08-17 | 哈尔滨工程大学 | A kind of method that freeze-drying prepares calcium alginate Biological gel membrane |
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| CN113429602A (en) * | 2021-06-23 | 2021-09-24 | 哈尔滨工程大学 | Preparation process method of sodium alginate/carboxymethyl cellulose actuating membrane |
| CN113527732A (en) * | 2021-06-30 | 2021-10-22 | 哈尔滨工程大学 | Preparation method of polyvinyl alcohol-sodium alginate gel actuating membrane |
| CN113571345A (en) * | 2021-06-30 | 2021-10-29 | 哈尔滨工程大学 | Preparation process method of manganese dioxide doped graphene oxide electrode film |
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