CN105153480B - A kind of method and application preparing its liquid crystalline phase by regulating and controlling sodium alginate molecular weight distribution - Google Patents
A kind of method and application preparing its liquid crystalline phase by regulating and controlling sodium alginate molecular weight distribution Download PDFInfo
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Abstract
The method that the invention discloses a kind of to prepare its liquid crystalline phase by regulating and controlling sodium alginate molecular weight distribution, includes the following steps：The sodium alginate of high molecular weight is obtained into the sodium alginate of low molecular weight by degradation；The sodium alginate of high molecular weight is mixed with the sodium alginate of low molecular weight, is then dissolved in deionized water, stirs to get uniform sodium alginate soln；Above-mentioned uniform sodium alginate soln is mutually separated by standing or being centrifuged to bring it about, taking lower layer is mutually sodium alginate liquid crystalline phase.The molecular weight that the present invention passes through simply regulation sodium alginate, without adding other electrolyte, pure sodium alginate liquid crystalline phase can be obtained, provide possibility for the preparation multi-functional sodium alginate material of anisotropy high-performance, method simplicity is quick, low in cost, environmentally friendly.
Description
Technical field
The present invention relates to a kind of methods and application that its liquid crystalline phase is prepared by regulating and controlling sodium alginate molecular weight distribution, belong to
Polymeric material field.
Background technique
Sodium alginate is to pass through one kind made of 1-4 glucosides key connection as beta-D-mannuronic acid and α-L- guluronic acid
Natural macromolecule amylose polymer is widely used in fiber due to its unique physicochemical property and good biocompatibility
In the various fields such as weaving, pharmaceutical preparation, food processing, organizational project.The one kind especially prepared using sodium alginate as raw material
Reproducibility resource new fiber materials, because it can be dropped with superpower essence from fire-retardant, high-hygroscopicity, certain radiation protection, biology
A series of excellent characteristics such as solution and bio-compatible receive significant attention, and have a extensive future.
However, it is worth mentioning that, liquid crystal behavior in relation to natural polysaccharide and its application have been carried out grinding extensively and profoundly
Study carefully, if cellulose, chitosan, hyaluronic acid have all obtained liquid crystalline phase, but the characteristics of due to sodium alginate structure, there is rigidity
Poor, the features such as G sections and M sections of strand are alternately arranged, it is more difficult to form liquid crystalline phase, therefore about alginic acid (salt) liquid crystal material and
The research of preparation method is rarely reported.It proposes to be added to sea with different electrolyte application No. is 2015102285128 patent
Liquid crystalline phase is obtained in solution of sodium alginate, but sodium alginate solution is influenced due to the electrolyte containing a large amount of non-sodium alginates in system
The further extensive use of crystal phase.
Summary of the invention
The method that the purpose of the present invention is to provide a kind of to prepare its liquid crystalline phase by regulating and controlling sodium alginate molecular weight distribution
And pure alginic acid can be obtained without adding other electrolyte by simply regulating and controlling the molecular weight of sodium alginate in application, this method
Sodium liquid crystalline phase provides possibility for the preparation multi-functional sodium alginate material of anisotropy high-performance.
The adopted technical solution is that：
A method of its liquid crystalline phase being prepared by regulating and controlling sodium alginate molecular weight distribution, is included the following steps：
(1) sodium alginate of high molecular weight is obtained into the sodium alginate of low molecular weight by degradation；
(2) sodium alginate of high molecular weight is mixed with the sodium alginate of low molecular weight, is then dissolved in deionization
In water, uniform sodium alginate soln is stirred to get；
(3) by above-mentioned uniform sodium alginate soln by standing or centrifugation brings it about and mutually separates, the lower layer is taken mutually to be
Sodium alginate liquid crystalline phase.
In step (1), sodium alginate is the natural biomass extracted from brown alga or bacterium, including different M/G composition
And the sodium alginate of the different molecular weight of degradation.
In step (1), degradation mode includes oxidative degradation, thermal degradation, ray degradation, enzyme degradation and ultrasonotomography etc..
Above-mentioned Oxidative Degradation Process includes the following steps：The sodium alginate powder for weighing high molecular weight is dissolved in deionized water
In be configured to the sodium alginate soln that mass percent concentration is 2%-10%, then heating water bath is added to 50 DEG C -60 DEG C
H2O2The mass fraction for accounting for sodium alginate soln to it is 0.5%-1%, 2-12h is stirred to react, after the reaction was completed according to alginic acid
Dehydrated alcohol is added in sodium solution/ethyl alcohol=1/2 volume ratio, the sodium alginate of low molecular weight is precipitated, using freeze-drying
48h-96h obtains the sodium alginate powder of low molecular weight.
It, can be by the product of the different degradation time sections of collection, to obtain two or more different low molecular weights in step (1)
Sodium alginate.
In step (2), the sodium alginate of high molecular weight refers to that molecular weight is greater than the sodium alginate of 150kDa；Low molecular weight
Sodium alginate refer to molecular weight be less than 150kDa sodium alginate.
In step (2), the mass ratio of the sodium alginate of the sodium alginate and low molecular weight of high molecular weight is 0.1-5.
In step (2), preferably by the sodium alginate of two or more different high molecular weight and two or more different low points
The sodium alginate of son amount is mixed.
In step (2), mixing time is preferably 2-12h.
In step (2), mass percent concentration≤70% of the uniform sodium alginate soln.
In step (3), uniform sodium alginate soln will occur mutually to separate by the standing or centrifugation of certain time, molecule
The time of the smaller standing of amount distribution or centrifugation is longer.
In step (3), lower layer's liquid crystalline phase has apparent liquid crystal texture in cross-polarized light polarized light microscopy microscopic observation.
The sodium alginate of high molecular weight described in the sodium alginate of high molecular weight described in step (1) and step (2)
Its molecular weight can be identical, can also be different.
Above-mentioned sodium alginate liquid crystalline phase can prepare the side such as high-performance fiber, highly oriented alginate films, gel
Face application.It can be applied in weaving, field of food and medicine from the point of view of wider.
The method have the benefit that：
1, the present invention carries out simple regulation by the molecular weight distribution to sodium alginate and has obtained the liquid crystal of sodium alginate
Phase, method simplicity are quick, low in cost, environmentally friendly.
2, the present invention does not need that liquid crystalline phase can be obtained by the way that other substances are added in sodium alginate aqueous solution, avoids
The influence of gained liquid crystal solution other substances in application process, to prepare the multi-functional sodium alginate material of anisotropy high-performance
Material provides possibility.
3, operation of the present invention is simple, and product is easily obtained, and is suitable for industrialized production.
Specific embodiment
The present invention is further illustrated combined with specific embodiments below.
Embodiment 1
H2O2The sodium alginate of oxidative degradation acquisition low molecular weight
Sodium alginate powder (250kDa) dissolution for weighing a certain amount of high molecular weight is configured to quality in deionized water
H is added to 80 DEG C in the sodium alginate soln that percent concentration is 2%, heating water bath2O2It is 0.25% to its mass fraction, stirring
Reaction time can be 2h, 4h, 6h, 8h, 10h (it is smaller that the reaction time gets over long molecule amount).Reach the reaction time after according to solution/
Dehydrated alcohol is added in the volume ratio of ethyl alcohol=1/2, and the sodium alginate of low molecular weight is precipitated, and obtains using freeze-drying 96h
Sodium alginate powder.Its molecular weight is characterized using GPC.Obtain molecular weight be 143kDa, 120kDa, 105kDa,
The sodium alginate of the low molecular weight of 90kDa, 80kDa.
The sodium alginate powder (80kDa) for weighing the above-mentioned low molecular weight of 10g is added in the deionized water of 87ml, and stirring 2h is equal
It is even to be configured to uniform solution.The sodium alginate (300kDa) for weighing 3g high molecular weight again is added in above-mentioned solution, stirs 2h, obtains
Obtain uniform sodium alginate soln.The centrifugation that above-mentioned uniform sodium alginate soln is passed through to 3h, 3000r/min obtains up and down
Different two-phases, take lower layer mutually be sodium alginate liquid crystalline phase.
Embodiment 2
The sodium alginate of thermal degradation acquisition low molecular weight
The sodium alginate powder (300kDa) for weighing four parts of 20g, be put into 180 DEG C of vacuum drying ovens distinguish thermal degradation 2h, 4h,
6h,8h.It by the sodium alginate powder after above-mentioned four parts degradations, is added in distilled water while stirring, stirs 2h, quality is made
The thermal degradation sodium alginate soln that percent concentration is 3%.By above-mentioned each sodium alginate soln with the speed of 13000r/min from
Heart 20min, the upper solution after taking centrifugation are placed in room temperature in baking oven and are evaporated to obtain the sodium alginate of four kinds of different low molecular weights
Powder.Its molecular weight is characterized using GPC.Obtain the low molecule that molecular weight is 150kDa, 120kDa, 100kDa, 90kDa
The sodium alginate of amount.
The sodium alginate powder (120kDa) for weighing the above-mentioned low molecular weight of 30g is added in the deionized water of 60ml, stirs 4h
Uniformly it is configured to uniform solution.It takes the sodium alginate (280kDa) of 10g high molecular weight to be added in above-mentioned uniform solution again, stirs
It mixes 2h and obtains uniform sodium alginate soln.The centrifugation that above-mentioned uniform sodium alginate soln is passed through to 6h, 3000r/min, obtains
To different two-phase up and down, lower layer is taken mutually and is the liquid crystalline phase of sodium alginate.
Embodiment 3
The sodium alginate of ultrasonotomography acquisition low molecular weight
The sodium alginate soln that various concentration are prepared with deionized water takes its 40mL merging to have in the container of energy converter,
Certain supersonic frequency and ultrasonic power are adjusted, ultrasonotomography is carried out, it is a small amount of to take out the solution in different ultrasonic times.Benefit
Its molecular weight is characterized with GPC.Obtain the sodium alginate for the low molecular weight that molecular weight is 80kDa.
The sodium alginate (80kDa) for weighing the above-mentioned low molecular weight of 2g is added in the deionized water of 93ml, and stirring 2h uniformly matches
Uniform solution is made.The sodium alginate (400kDa) of 5g high molecular weight is taken to be added in above-mentioned uniform solution again, stirring 2h is obtained
Obtain uniform sodium alginate soln.The centrifugation that above-mentioned uniform sodium alginate soln is passed through to 2h, 3000r/min obtains up and down
Different two-phases, take lower layer mutually be sodium alginate liquid crystalline phase.
Embodiment 4
The sodium alginate of irradiation-induced degradation acquisition low molecular weight
Sodium alginate (350kDa) aqueous solution that configuration quality percent concentration is 5%, is put into60Spoke in Co γ irradiation field
According to absorbed dose rate is 80Gy/min, and absorbed dose is respectively 15,25,40,60kGy.After the completion of irradiation, by sample in 5O
It is dried at DEG C.Its molecular weight is characterized using GPC.Obtaining molecular weight is 140kDa, 130kDa, 120kDa, 112kDa
The sodium alginate of low molecular weight.
The sodium alginate (120kDa) for weighing the above-mentioned low molecular weight of 5g is added in the deionized water of 90ml, and stirring 2h uniformly matches
Uniform solution is made.The sodium alginate (350kDa) for weighing 5g high molecular weight again is added in above-mentioned uniform solution, stirs 2h,
Obtain uniform sodium alginate soln.The centrifugation that above-mentioned uniform sodium alginate soln is passed through to 2h, 3000r/min, obtains
Lower different two-phase, take lower layer mutually be sodium alginate liquid crystalline phase.
Embodiment 5
The sodium alginate of microbial degradation acquisition low molecular weight
Configuration quality percent concentration be 3% sodium alginate (400kDa) aqueous solution, be put into certain microorganism (such as
Alginic acid bacterium), carry out the stirring of 10h, 20h, 40h, 60h respectively at 25 DEG C.Pass through 3000r/min after the completion of degradation, 2h's
It is centrifugated out microorganism, sodium alginate sample is dried at 5O DEG C.Its molecular weight is characterized using GPC.Divided
Son amount is the sodium alginate of the low molecular weight of 145kDa, 130kDa, 100kDa, 75kDa.
The SA for weighing the above-mentioned low molecular weight of 0.5g (75kDa) is added in the deionized water of 99.2ml, and stirring 1h is uniformly prepared
At uniform solution.The sodium alginate (400kDa) of 0.3g high molecular weight is taken to be added in above-mentioned uniform solution again, stirring 2h is obtained
Obtain uniform sodium alginate soln.The centrifugation that above-mentioned uniform sodium alginate soln is passed through to 1h, 3000r/min obtains up and down
Different two-phases, take lower layer mutually be sodium alginate liquid crystalline phase.
Embodiment 6
SA and the 1g molecular weight for weighing 1g molecular weight 100kDa are that the deionized water of 98.8ml is added in the SA of 80kDa together
In, stirring 1h is uniformly configured to uniform solution.The sodium alginate of 0.2g molecular weight 500kDa is taken to be with 0.5g molecular weight again
The sodium alginate of 400kDa is added in above-mentioned uniform solution, and stirring 2h obtains uniform sodium alginate soln.It will be above-mentioned uniform
Sodium alginate soln pass through the centrifugation of 2h, 3000r/min, obtain different two-phase up and down, taking lower layer is mutually sodium alginate
Liquid crystalline phase.
Embodiment 7
It weighs the SA that 4g molecular weight is 100kDa and the deionized water of 92.0ml is added in the SA that 1g molecular weight is 80kDa together
In, stirring 1h is uniformly configured to uniform solution.The sodium alginate that 3g molecular weight is 350kDa is taken to be with 0.5g molecular weight again
The sodium alginate of 500Kda is added in above-mentioned uniform solution, and stirring 2h obtains uniform sodium alginate soln.It will be above-mentioned uniform
Sodium alginate soln pass through the centrifugation of 4h, 8000r/min, obtain different two-phase up and down, taking lower layer is mutually sodium alginate
Liquid crystalline phase.
Claims (4)
1. a kind of method for preparing its liquid crystalline phase by regulating and controlling sodium alginate molecular weight distribution, it is characterised in that including following step
Suddenly：
(1) the sodium alginate A of high molecular weight is degraded, the sodium alginate of low molecular weight is made；
(2) then, the sodium alginate dissolution for weighing low molecular weight in deionized water, stirs and is configured to uniform solution C；
The sodium alginate B for weighing high molecular weight is added in above-mentioned uniform solution C, is stirred 2-12h, is obtained uniform quality percentage
Specific concentration is the sodium alginate soln D of 0.8%-40%；The sodium alginate B of the high molecular weight and the sodium alginate of low molecular weight
Mass ratio is 0.1-5；
The sodium alginate A of above-mentioned high molecular weight refers to that molecular weight is the sodium alginate of 250kDa-400kDa, the sea of high molecular weight
Mosanom B refers to that molecular weight is the sodium alginate of 280kDa-500kDa, and the sodium alginate of low molecular weight refers to that molecular weight is
The sodium alginate of 80kDa-150kDa；
(3) gained sodium alginate soln D is brought it about by centrifugation and is mutually separated, taking lower layer is mutually sodium alginate liquid crystalline phase.
2. the method according to claim 1 for preparing its liquid crystalline phase by regulating and controlling sodium alginate molecular weight distribution, feature
It is, degradation mode includes oxidative degradation, thermal degradation, ray degradation, enzyme degradation or ultrasonotomography.
3. the method according to claim 1 for preparing its liquid crystalline phase by regulating and controlling sodium alginate molecular weight distribution, feature
It is, the oxidative degradation includes the following steps：The sodium alginate A powder dissolution for weighing high molecular weight is prepared in deionized water
Then H is added to 50 DEG C -60 DEG C in the sodium alginate soln for being 2%-10% at mass percent concentration, heating water bath2O2To it
Account for sodium alginate soln mass fraction be 0.5%-1%, be stirred to react 2-12h, after the reaction was completed according to sodium alginate soln/
Dehydrated alcohol is added in the volume ratio of ethyl alcohol=1/2, is precipitated, and using freeze-drying 48h-96h, obtains the low molecule of powdered form
The sodium alginate of amount.
4. such as the method as claimed in any one of claims 1-3 for preparing its liquid crystalline phase by regulating and controlling sodium alginate molecular weight distribution,
It is characterized in that, the sodium alginate liquid crystalline phase, can be used for high-performance sodium alginate fiber, highly oriented alginate films or
The preparation of sodium alginate gel.
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| CN113004434B (en) * | 2021-03-03 | 2022-11-11 | 大连工业大学 | Sodium alginate degradation method based on bismuth tungstate photocatalyst |
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| 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 |
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| 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 |
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