CN105153480A - Method for preparing sodium alginate liquid crystalline phase through regulation and control of molecular weight distribution of sodium alginate, as well as application of sodium alginate liquid crystalline phase - Google Patents
Method for preparing sodium alginate liquid crystalline phase through regulation and control of molecular weight distribution of sodium alginate, as well as application of sodium alginate liquid crystalline phase Download PDFInfo
- Publication number
- CN105153480A CN105153480A CN201510648304.3A CN201510648304A CN105153480A CN 105153480 A CN105153480 A CN 105153480A CN 201510648304 A CN201510648304 A CN 201510648304A CN 105153480 A CN105153480 A CN 105153480A
- Authority
- CN
- China
- Prior art keywords
- sodium alginate
- molecular
- molecular weight
- regulation
- mesomorphic phase
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Medicinal Preparation (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention discloses a method for preparing a sodium alginate liquid crystalline phase through regulation and control of molecular weight distribution of sodium alginate. The method comprises the following steps: degrading sodium alginate with high molecular weight to obtain sodium alginate with low molecular weight; mixing sodium alginate with high molecular weight and sodium alginate with low molecular weight, then dissolving the mixture to deionized water, and stirring to obtain a uniform sodium alginate solution; conducting still standing or centrifugation on the uniform sodium alginate solution for phase separation, and taking the lower layer phase as the sodium alginate liquid crystalline phase. According to the method, the pure sodium alginate liquid crystalline phase can be obtained by simple regulation and control of the molecular weight of sodium alginate without addition of other electrolytes, possibility is provided for preparation of sodium alginate material with high anisotropy and performance and multiple functions, and the method is simple, quick, low in cost and environment-friendly.
Description
Technical field
The present invention relates to a kind of method and the application of being prepared its mesomorphic phase by regulation and control sodium alginate molecular weight distribution, belong to polymeric material field.
Background technology
Sodium alginate is a kind of natural macromolecule amylose polymkeric substance be formed by connecting by 1-4 glycosidic link by beta-D-mannuronic acid and α-L-guluronic acid, due to physicochemical property and the good biocompatibility of its uniqueness, be widely used in the various fields such as fibrous woven, pharmaceutical preparation, food-processing, organizational project.It is particularly a kind of recyclability resource new fiber materials prepared by raw material with sodium alginate, be subject to extensive concern because it has superpower essence from a series of excellent specific properties such as fire-retardant, high-hygroscopicity, certain radioprotective, biodegradable and physiologically acceptable, have a extensive future.
But, what be worth proposition is, about natural polysaccharide liquid crystal behavior and application carried out research extensively and profoundly, as Mierocrystalline cellulose, chitosan, hyaluronic acid obtain mesomorphic phase all, but due to the feature of sodium alginate structure, have that rigidity is poor, the feature such as molecular chain G section and M section are alternately arranged, more difficult formation mesomorphic phase, the research therefore about Lalgine (salt) liquid crystal material and preparation method thereof rarely has report.Application number be 2015102285128 patent propose to add in sodium alginate soln with different ionogen to obtain mesomorphic phase, but due to the ionogen containing a large amount of non-sodium alginate in system, affect the further widespread use of sodium alginate mesomorphic phase.
Summary of the invention
The object of the present invention is to provide a kind of method and the application of being prepared its mesomorphic phase by regulation and control sodium alginate molecular weight distribution, the method is by the molecular weight of simple regulation and control sodium alginate, without the need to adding other ionogen, pure sodium alginate mesomorphic phase can be obtained, for the multi-functional sodium alginate material of preparation anisotropy high-performance provides possibility.
The technology used in the present invention solution is:
Prepared a method for its mesomorphic phase by regulation and control sodium alginate molecular weight distribution, comprise the following steps:
(1) sodium alginate of high molecular is obtained low-molecular-weight sodium alginate by degraded;
(2) sodium alginate of high molecular is mixed with low-molecular-weight sodium alginate, then dissolve in deionized water, stir and obtain homogeneous sodium alginate soln;
(3) make it be separated through standing or centrifugal above-mentioned homogeneous sodium alginate soln, take off layer and be sodium alginate mesomorphic phase mutually.
In step (1), sodium alginate is the natural biomass extracted from brown alga or bacterium, comprises the sodium alginate of the different molecular weight of different M/G composition and degraded.
In step (1), degraded mode comprises oxidative degradation, thermal destruction, ray degraded, enzyme liberating and ultrasonic degradation etc.
Above-mentioned Oxidative Degradation Process comprises the following steps: the sodium alginate powder taking high molecular dissolves and is mixed with the sodium alginate soln that mass percent concentration is 2%-10% in deionized water, and heating in water bath, to 50 DEG C-60 DEG C, then adds H
2o
2be 0.5%-1% to its massfraction accounting for sodium alginate soln, stirring reaction 2-12h, dehydrated alcohol is added according to the volume ratio of sodium alginate soln/ethanol=1/2 after having reacted, separate out low-molecular-weight sodium alginate, again through lyophilize 48h-96h, obtain low-molecular-weight sodium alginate powder.
In step (1), by collecting the product of different degradation time section, to obtain the low-molecular-weight sodium alginate of two or more difference.
In step (2), the sodium alginate of high molecular refers to the sodium alginate that molecular weight is greater than 150kDa; Low-molecular-weight sodium alginate refers to the sodium alginate that molecular weight is less than 150kDa.
In step (2), the sodium alginate of high molecular and the mass ratio of low-molecular-weight sodium alginate are 0.1-5.
In step (2), preferably the sodium alginate of two or more different high molecular is mixed from two or more different low-molecular-weight sodium alginate.
In step (2), churning time is preferably 2-12h.
In step (2), mass percent concentration≤70% of described homogeneous sodium alginate soln.
In step (3), homogeneous sodium alginate soln will be separated through the standing or centrifugal of certain hour, and the molecular weight distribution less standing or centrifugal time is longer.
In step (3), subnatant crystalline phase, at cross-polarized light polarized light microscopy Microscopic observation, has obvious liquid crystal texture.
The sodium alginate of the high molecular described in step (1) can be identical with its molecular weight of sodium alginate of the high molecular described in step (2), also can be different.
Above-mentioned sodium alginate mesomorphic phase can be applied in the alginate films, gel etc. of preparing high-performance fiber, high orientation.Widerly can to apply in weaving, food, field of medicaments.
Advantageous Effects of the present invention is:
1, the present invention obtains the mesomorphic phase of sodium alginate by carrying out simple regulation and control to the molecular weight distribution of sodium alginate, and method is easy to be quick, with low cost, environmentally friendly.
2, the present invention does not need can obtain mesomorphic phase by adding other materials in sodium alginate aqueous solution, avoid the impact of gained liquid crystal solution other materials in application process, for the multi-functional sodium alginate material of preparation anisotropy high-performance provides possibility.
3, the present invention is simple to operate, and product is easy to obtain, and is suitable for suitability for industrialized production.
Embodiment
Below in conjunction with specific embodiment, the present invention is further illustrated.
Embodiment 1
H
2o
2oxidative degradation obtains low-molecular-weight sodium alginate
The sodium alginate powder (250kDa) taking a certain amount of high molecular dissolves and is mixed with the sodium alginate soln that mass percent concentration is 2% in deionized water, and heating in water bath, to 80 DEG C, adds H
2o
2be 0.25% to its massfraction, the stirring reaction time can be 2h, 4h, 6h, 8h, 10h (reaction times, longer molecular weight was less).Add dehydrated alcohol according to the volume ratio of solution/ethanol=1/2 after arriving the reaction times, separate out low-molecular-weight sodium alginate, then obtain sodium alginate powder through lyophilize 96h.GPC is utilized to characterize its molecular weight.Obtain the low-molecular-weight sodium alginate that molecular weight is 143kDa, 120kDa, 105kDa, 90kDa, 80kDa.
Taking the above-mentioned low-molecular-weight sodium alginate powder (80kDa) of 10g adds in the deionized water of 87ml, stirs 2h and is evenly mixed with homogeneous solution.The sodium alginate (300kDa) taking 3g high molecular again adds in above-mentioned solution, stirs 2h, obtains homogeneous sodium alginate soln.By centrifugal through 3h, 3000r/min of above-mentioned homogeneous sodium alginate soln, obtain two-phases different up and down, take off the mesomorphic phase that layer is sodium alginate mutually.
Embodiment 2
Thermal destruction obtains low-molecular-weight sodium alginate
Take the sodium alginate powder (300kDa) of four parts of 20g, put into 180 DEG C of vacuum drying ovens thermal destruction 2h, 4h, 6h, 8h respectively.By the sodium alginate powder after above-mentioned four parts of degradeds, join while stirring in distilled water, stir 2h, all make the thermal destruction sodium alginate soln that mass percent concentration is 3%.By above-mentioned each sodium alginate soln with the centrifugation 20min of 13000r/min, get centrifugal after upper solution be placed in baking oven normal temperature evaporate to dryness and obtain four kinds of different low-molecular-weight sodium alginate powders.GPC is utilized to characterize its molecular weight.Obtain the low-molecular-weight sodium alginate that molecular weight is 150kDa, 120kDa, 100kDa, 90kDa.
Taking the above-mentioned low-molecular-weight sodium alginate powder (120kDa) of 30g adds in the deionized water of 60ml, stirs 4h and is evenly mixed with homogeneous solution.The sodium alginate (280kDa) getting 10g high molecular again adds in above-mentioned homogeneous solution, stirs 2h and obtains homogeneous sodium alginate soln.By centrifugal through 6h, 3000r/min of above-mentioned homogeneous sodium alginate soln, obtain two-phases different up and down, take off the mesomorphic phase that layer is sodium alginate mutually.
Embodiment 3
Ultrasonic degradation obtains low-molecular-weight sodium alginate
Prepare the sodium alginate soln of various concentration with deionized water, get in container that its 40mL inserts with transverter, regulate certain ultrasonic frequency and ultrasonic power, carry out ultrasonic degradation, take out this solution when different ultrasonic times a small amount of.GPC is utilized to characterize its molecular weight.Obtain the low-molecular-weight sodium alginate that molecular weight is 80kDa.
Taking the above-mentioned low-molecular-weight sodium alginate (80kDa) of 2g adds in the deionized water of 93ml, stirs 2h and is evenly mixed with homogeneous solution.The sodium alginate (400kDa) getting 5g high molecular again adds in above-mentioned homogeneous solution, stirs 2h and obtains homogeneous sodium alginate soln.By centrifugal through 2h, 3000r/min of above-mentioned homogeneous sodium alginate soln, obtain two-phases different up and down, take off the mesomorphic phase that layer is sodium alginate mutually.
Embodiment 4
Irradiation-induced degradation obtains low-molecular-weight sodium alginate
Configuration quality percentage concentration is sodium alginate (350kDa) aqueous solution of 5%, puts into
60irradiation in Co γ irradiation field, absorbed dose rate is 80Gy/min, absorption dose is respectively 15,25,40,60kGy.After irradiation completes, sample is dried at 5O DEG C.GPC is utilized to characterize its molecular weight.Obtain the low-molecular-weight sodium alginate that molecular weight is 140kDa, 130kDa, 120kDa, 112kDa.
Taking the above-mentioned low-molecular-weight sodium alginate (120kDa) of 5g adds in the deionized water of 90ml, stirs 2h and is evenly mixed with homogeneous solution.The sodium alginate (350kDa) taking 5g high molecular again adds in above-mentioned homogeneous solution, stirs 2h, obtains homogeneous sodium alginate soln.By centrifugal through 2h, 3000r/min of above-mentioned homogeneous sodium alginate soln, obtain two-phases different up and down, take off the mesomorphic phase that layer is sodium alginate mutually.
Embodiment 5
Microbiological deterioration obtains low-molecular-weight sodium alginate
Configuration quality percentage concentration is sodium alginate (400kDa) aqueous solution of 3%, puts into certain microorganism (such as alginic acid bacterium), carries out the stirring of 10h, 20h, 40h, 60h at 25 DEG C respectively.Centrifugation by 3000r/min, 2h after having degraded goes out microorganism, is dried by sodium alginate sample at 5O DEG C.GPC is utilized to characterize its molecular weight.Obtain the low-molecular-weight sodium alginate that molecular weight is 145kDa, 130kDa, 100kDa, 75kDa.
The SA taking the above-mentioned lower molecular weight of 0.5g (75kDa) adds in the deionized water of 99.2ml, stirs 1h and is evenly mixed with homogeneous solution.The sodium alginate (400kDa) getting 0.3g high molecular again adds in above-mentioned homogeneous solution, stirs 2h and obtains homogeneous sodium alginate soln.By centrifugal through 1h, 3000r/min of above-mentioned homogeneous sodium alginate soln, obtain two-phases different up and down, take off the mesomorphic phase that layer is sodium alginate mutually.
Embodiment 6
SA and the 1g molecular weight taking 1g molecular weight 100kDa is that the SA of 80kDa adds in the deionized water of 98.8ml in the lump, stirs 1h and is evenly mixed with homogeneous solution.Getting the sodium alginate of 0.2g molecular weight 500kDa and 0.5g molecular weight is again that the sodium alginate of 400kDa adds in above-mentioned homogeneous solution, stirs 2h and obtains homogeneous sodium alginate soln.By centrifugal through 2h, 3000r/min of above-mentioned homogeneous sodium alginate soln, obtain two-phases different up and down, take off the mesomorphic phase that layer is sodium alginate mutually.
Embodiment 7
To take 4g molecular weight be SA and the 1g molecular weight of 100kDa is that the SA of 80kDa adds in the deionized water of 92.0ml in the lump, stirs 1h and is evenly mixed with homogeneous solution.Getting sodium alginate that 3g molecular weight is 350kDa and 0.5g molecular weight is again that the sodium alginate of 500Kda adds in above-mentioned homogeneous solution, stirs 2h and obtains homogeneous sodium alginate soln.By centrifugal through 4h, 8000r/min of above-mentioned homogeneous sodium alginate soln, obtain two-phases different up and down, take off the mesomorphic phase that layer is sodium alginate mutually.
Claims (10)
1. prepared a method for its mesomorphic phase by regulation and control sodium alginate molecular weight distribution, it is characterized in that comprising the following steps:
(1) sodium alginate of high molecular is obtained low-molecular-weight sodium alginate by degraded;
(2) sodium alginate of high molecular is mixed with low-molecular-weight sodium alginate, then dissolve in deionized water, stir and obtain homogeneous sodium alginate soln;
(3) make it be separated through standing or centrifugal above-mentioned homogeneous sodium alginate soln, take off layer and be sodium alginate mesomorphic phase mutually.
2. a kind of method being prepared its mesomorphic phase by regulation and control sodium alginate molecular weight distribution according to claim 1, be is characterized in that, in step (1), degraded mode comprises oxidative degradation, thermal destruction, ray degraded, enzyme liberating and ultrasonic degradation.
3. a kind of method being prepared its mesomorphic phase by regulation and control sodium alginate molecular weight distribution according to claim 1, it is characterized in that, in step (1), by collecting the product of different degradation time section, to obtain the low-molecular-weight sodium alginate of two or more difference.
4. a kind of method being prepared its mesomorphic phase by regulation and control sodium alginate molecular weight distribution according to claim 2, it is characterized in that, described Oxidative Degradation Process comprises the following steps: the sodium alginate powder taking high molecular dissolves and is mixed with the sodium alginate soln that mass percent concentration is 2%-10% in deionized water, heating in water bath, to 50 DEG C-60 DEG C, then adds H
2o
2be 0.5%-1% to its massfraction accounting for sodium alginate soln, stirring reaction 2-12h, dehydrated alcohol is added according to the volume ratio of sodium alginate soln/ethanol=1/2 after having reacted, separate out low-molecular-weight sodium alginate, again through lyophilize 48h-96h, obtain low-molecular-weight sodium alginate powder.
5. a kind of method being prepared its mesomorphic phase by regulation and control sodium alginate molecular weight distribution according to claim 1, be is characterized in that, in step (2), the sodium alginate of high molecular refers to the sodium alginate that molecular weight is greater than 150kDa; Low-molecular-weight sodium alginate refers to the sodium alginate that molecular weight is less than 150kDa.
6. a kind of method being prepared its mesomorphic phase by regulation and control sodium alginate molecular weight distribution according to claim 1, it is characterized in that, in step (2), the sodium alginate of high molecular and the mass ratio of low-molecular-weight sodium alginate are 0.1-5.
7. a kind of method being prepared its mesomorphic phase by regulation and control sodium alginate molecular weight distribution according to claim 1, it is characterized in that, in step (2), the sodium alginate of two or more different high molecular is mixed from two or more different low-molecular-weight sodium alginate.
8. a kind of method being prepared its mesomorphic phase by regulation and control sodium alginate molecular weight distribution according to claim 1, it is characterized in that, in step (2), churning time is 2-12h.
9. a kind of method being prepared its mesomorphic phase by regulation and control sodium alginate molecular weight distribution according to claim 1, be is characterized in that, in step (2), and mass percent concentration≤70% of described homogeneous sodium alginate soln.
10. the sodium alginate mesomorphic phase as described in claim arbitrary in claim 1-9 is preparing the application in high-performance fiber, the alginate films of high orientation, gel.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510648304.3A CN105153480B (en) | 2015-10-09 | 2015-10-09 | A kind of method and application preparing its liquid crystalline phase by regulating and controlling sodium alginate molecular weight distribution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510648304.3A CN105153480B (en) | 2015-10-09 | 2015-10-09 | A kind of method and application preparing its liquid crystalline phase by regulating and controlling sodium alginate molecular weight distribution |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105153480A true CN105153480A (en) | 2015-12-16 |
| CN105153480B CN105153480B (en) | 2018-11-16 |
Family
ID=54794551
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510648304.3A Active CN105153480B (en) | 2015-10-09 | 2015-10-09 | A kind of method and application preparing its liquid crystalline phase by regulating and controlling sodium alginate molecular weight distribution |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105153480B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106498559A (en) * | 2016-09-23 | 2017-03-15 | 青岛大学 | A kind of method that use small-molecular-weight sodium alginate is self-assembled into nanofiber |
| CN109264766A (en) * | 2018-09-29 | 2019-01-25 | 青岛大学 | A kind of one kettle way preparation of different-shape nano particle |
| CN113004434A (en) * | 2021-03-03 | 2021-06-22 | 大连工业大学 | Sodium alginate degradation method based on bismuth tungstate photocatalyst |
| CN113307533A (en) * | 2021-06-15 | 2021-08-27 | 广东龙腾建材科技有限公司 | Special early strength water reducing agent for highway and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103694488A (en) * | 2013-12-18 | 2014-04-02 | 青岛大学 | Preparation method and application of alginic acid or alginate liquid crystal film |
| CN104861217A (en) * | 2015-05-07 | 2015-08-26 | 青岛大学 | Method for preparing alginate liquid crystalline phases |
-
2015
- 2015-10-09 CN CN201510648304.3A patent/CN105153480B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103694488A (en) * | 2013-12-18 | 2014-04-02 | 青岛大学 | Preparation method and application of alginic acid or alginate liquid crystal film |
| CN104861217A (en) * | 2015-05-07 | 2015-08-26 | 青岛大学 | Method for preparing alginate liquid crystalline phases |
Non-Patent Citations (1)
| Title |
|---|
| 左榘；马先；姬昂: "海藻酸钠热稳定性研究", 《南开大学学报》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106498559A (en) * | 2016-09-23 | 2017-03-15 | 青岛大学 | A kind of method that use small-molecular-weight sodium alginate is self-assembled into nanofiber |
| CN109264766A (en) * | 2018-09-29 | 2019-01-25 | 青岛大学 | A kind of one kettle way preparation of different-shape nano particle |
| CN113004434A (en) * | 2021-03-03 | 2021-06-22 | 大连工业大学 | Sodium alginate degradation method based on bismuth tungstate photocatalyst |
| CN113307533A (en) * | 2021-06-15 | 2021-08-27 | 广东龙腾建材科技有限公司 | Special early strength water reducing agent for highway and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105153480B (en) | 2018-11-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105153480A (en) | Method for preparing sodium alginate liquid crystalline phase through regulation and control of molecular weight distribution of sodium alginate, as well as application of sodium alginate liquid crystalline phase | |
| CN104558677A (en) | Preparation method of nano cellulose/chitosan composite foam | |
| CN105153438A (en) | Preparation method of high-strength high-swelling nanocellulose and polyving akohol composite hydrogel | |
| CN103788217B (en) | A kind of cellulose gel glue material, Preparation method and use | |
| CN103087516B (en) | Preparation method of nylon 6 and natural fiber composite material | |
| CN103028117A (en) | Method for preparing bacterial cellulose gel composite material | |
| CN104262493A (en) | Preparation method and use of medicinal pregelatinized hydroxypropyl starch | |
| CN102349863A (en) | Preparation method of algal polysaccharides toner | |
| CN104911230A (en) | Bacterial cellulose in-situ fermentation production method | |
| CN102634040B (en) | Basic solvent for dissolving chitosan and method for dissolving chitosan under alkaline condition | |
| CN102329422A (en) | Method for preparing chitosan grafted polylactic acid in ionic liquid | |
| CN101735394B (en) | Low monomer residue gardon asparagus superstrong water absorber and microwave radiation preparation method thereof | |
| CN102838683B (en) | Low molecular weight (LMW) xanthan gum and preparation method thereof | |
| CN104448145A (en) | Preparation method of super absorbent resin | |
| CN109402106A (en) | A kind of method and its application of the fixed Klebsiella of polyvinyl alcohol-cellulose | |
| CN102585255A (en) | Pectin/cellulose hydrogel material and preparation method thereof | |
| CN104403136A (en) | Medical pectin/bacterial cellulose composite film and preparation method thereof | |
| CN105713098A (en) | Method for preparing sodium carboxymethyl cellulose by fermenting bagasse | |
| CN101381479A (en) | Method for synthesizing alkaline soluble glycol cellulose for spinning/membrane manufacturing | |
| CN109266358A (en) | A kind of agricultural anti-drought water-retaining agent and preparation method thereof | |
| CN102276733A (en) | Method for preparing ethyl cellulose with high degree of substitution | |
| CN110041444B (en) | The preparation method of the modified xantham gum of oil and gas well fracturing fluid | |
| CN109535486B (en) | Method for preparing high-viscosity nanofiber gel by using celery | |
| CN107722196B (en) | method for preparing weathered coal humic acid-based super absorbent resin by aqueous solution polymerization method | |
| CN105002582A (en) | Preparation method of Chinese mugwort cellulose spinning solution |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |