CN106565852A - Sodium alginate degradation method - Google Patents
Sodium alginate degradation method Download PDFInfo
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- CN106565852A CN106565852A CN201510647647.8A CN201510647647A CN106565852A CN 106565852 A CN106565852 A CN 106565852A CN 201510647647 A CN201510647647 A CN 201510647647A CN 106565852 A CN106565852 A CN 106565852A
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Abstract
The invention belongs to the technical field of polysaccharide degradation, and relates to a sodium alginate degradation method, which is characterized by comprising: 1) dispersing sodium alginate in an alcohol solution, adding an acid solution under a stirring condition, carrying out a reflux reaction under a thermal insulation state, stirring, and controlling the degradation time so as to complete the degradation reaction; 2) filtering the reaction system obtained in the step 1), washing the solid sequentially with deionized water and 75% ethanol to achieve a neutral state, dispersing in 75% ethanol, adding a sodium hydroxide solution under stirring, and adjusting the pH value of the system to more than or equal to 7; and 3) filtering the reaction system obtained in the step 2), washing the solid with 75% ethanol to achieve a neutral state, washing sequentially with 75% ethanol, 95% ethanol and dehydrated alcohol, dewatering, and carrying out vacuum drying to obtain the degraded sodium alginate product. According to the present invention, the method has advantages of convenient operation, simple preparation technology process, low manufacturing cost, and the like; the sodium alginate is dispersed in the blending liquid of the alcohol and the acid to carry out the heterogeneous degradation reaction so as to conveniently separate the product at the late stage; and the obtained degraded sodium alginate is the white or light yellow solid powder, and is dissolved in water to form the viscous liquid.
Description
Technical field
The present invention relates to a kind of biodegrading process of sodium alginate in polysaccharide degradation technique field.
Background technology
Sodium alginate, also known as Algin, is a kind of natural polysaccharide, and it, by the block linear polymer of β-D-1,4- mannuronic acids and α-L-1,4- two kinds of monomer compositions of guluronic acid, is white or pale yellow powder to be.There is sodium alginate antitumor, regulation immunocompetence, elimination free radical and antioxidation, lipidemia, reduction blood glucose, opposing radiation to play the effect such as protection effect, gelling ability with good biocompatibility and uniqueness, has blood coagulation resisting function to can be used to treat cardiovascular disease in vivo；There is anastalsis in vitro, can be used to develop external medical dressing.
The molecular weight of sodium alginate is up to several ten million, the sodium alginate degradation in vivo speed of high molecular is low, and the enzyme of sodium alginate of not degrading in vivo, and the sodium alginate of low-molecular-weight can slowly be discharged from organism in metabolism, and the sodium alginate oligosaccharide of low-molecular-weight can improve Keratiocyte growth rate, promote endothelial cell growth migration, promote fibroblast proliferation etc..Meanwhile, it is all relevant with molecular weight of high polymer that the Properties of Polymer such as polysaccharide are particularly mechanical performance, processing characteristics and macromolecule characteristic in the solution etc..
At present, it has been disclosed that degraded sodium alginate method mainly have acid degradation, enzymatic degradation, H2O2 oxidative degradations etc..For example：Kamal H. Bouhadir etc. disclose a kind of method of utilization concentrated hydrochloric acid in 2.85 times degraded sodium alginates of pH, are separated out using ethanol precipitation after being dissolved in sodium hydrate aqueous solution；V é ronique Breguet etc. disclose a kind of method degraded to sodium alginate by utilization alginate lyase, and detect sodium alginate degree of degradation with thiobarbituricacidα- method；Li Xiaoxia etc. discloses a kind of method that employing H2O2 carries out oxidative degradation to sodium alginate, has obtained the sodium alginate of low-molecular-weight.
It is wayward and the problems such as be not readily separated in view of existing these methods still suffer from degrading high cost, catabolite, to make up the deficiency of prior art, special invention this patent.
The content of the invention
It is an object of the invention to provide a kind of method of new degraded sodium alginate, realizes that under heterogeneous conditions sodium alginate is degraded, partial reaction liquid recoverable, this method can solve the problems, such as that degraded high cost, catabolite are not readily separated.The degraded sodium alginate for obtaining is white or faint yellow solid powder, is dissolved in water and forms thick liquid.
The present invention is by sodium alginate is dispersed in blended liquid of the alcohol with acid, realize that sodium alginate is reacted with the acid of liquid phase under solid phase, the present invention has the advantages that easy to operate, preparing technique process is easy and cheap for manufacturing cost, heterogeneous degradation reaction is carried out by sodium alginate is dispersed in blended liquid of the alcohol with acid, facilitates later product to separate.By controlling response time and reaction temperature, the sodium alginate of different molecular weight can be obtained.Same sodium alginate raw material, under fixed reaction temperature, can obtain the relation curve of molecular weight and response time, the sodium alginate for preparing molecular weight is repeated according to curve.
The present invention's concretely comprises the following steps：
1）Sodium alginate is scattered in alcoholic solution, acid solution is added thereto under agitation, the back flow reaction under keeping warm mode, stirring control degradation time, complete degradation reaction；
2）By step 1）The reaction system filtration of gained, deionized water, 75% ethanol are washed till neutrality to solid successively, are then dispersed in 75% ethanol, and stirring is lower to add sodium hydroxide solution, and regulation system pH is to more than or equal to 7；
3）By step 2）The reaction system of gained is filtered, after gained solid is Jing 75% washing with alcohol to neutrality, successively with 75%, 95%, absolute ethanol washing, dehydration, vacuum drying obtains sodium alginate product of degrading.
It is a feature of the present invention that concrete steps 1）Used in alcohol can be ethanol, ethylene glycol, normal propyl alcohol, isopropanol or methanol, the concentration of alcoholic solution is 5-24 mol/Ls, and its consumption can be 40-60 times of sodium alginate（g/ml）；The acid for being used can be concentrated hydrochloric acid, phosphoric acid or acetic acid, and the concentration of acid solution is 10-17 mol/Ls, and its consumption can be 3-20 times of sodium alginate（g/ml)；Reflux temperature can be 30-80 DEG C；Response time can be 0.5-48 hour.
The present invention is made below in conjunction with drawings and Examples and being further illustrated.
Description of the drawings
Relation curves of the Fig. 1 for sodium alginate molecular weight that viscosity-average molecular weight is 50,075,000 dalton and degradation time.
Specific embodiment
The present invention is further elaborated below by way of specific embodiment.
Embodiment 1
By 1 part（g）Initial viscosity-average molecular weight is that the sodium alginate of 50,075,000 dalton is scattered in 40 parts（ml）In 13 mol/L ethanol solution, stirring is lower to add 20 parts of the hydrochloric acid solution that molar concentration is 12 mol/Ls（ml）Back flow reaction 48 hours at 50 DEG C, reaction system is filtered, filtering residue is washed to neutrality Jing deionized water, 75% ethanol solution, is scattered in 75% ethanol solution, Deca sodium hydroxide solution, conciliation system pH is to more than or equal to 7, by the sodium alginate suspension sucking filtration for obtaining, after filtering residue is Jing 75% washing with alcohol to neutrality, graded ethanol is used（75%th, 95%, dehydrated alcohol）Washing, dehydration.It is vacuum dried at 60 DEG C.Sodium alginate Jing Ubbelohdes viscosimetry after degraded is determined, and viscosity-average molecular weight is 2,068,400 dalton.
Embodiment 2
By 1 part（g）Initial viscosity-average molecular weight is that the sodium alginate of 59,095,000 dalton is scattered in 45 parts（ml）In 24 mol/L methanol solutions, stirring is lower to add 15 parts of the phosphoric acid solution that molar concentration is 14 mol/Ls（ml）Back flow reaction 24 hours at 80 DEG C, reaction system is filtered, filtering residue is washed to neutrality Jing deionized water, 75% ethanol solution, is scattered in 75% ethanol solution, Deca sodium hydroxide solution, conciliation system pH is to more than or equal to 7, by the sodium alginate suspension sucking filtration for obtaining, after filtering residue is Jing 75% washing with alcohol to neutrality, graded ethanol is used（75%th, 95%, dehydrated alcohol）Washing, dehydration.It is vacuum dried at 60 DEG C.Sodium alginate Jing Ubbelohdes viscosimetry after degraded is determined, and viscosity-average molecular weight is 10,172,200 dalton.
Embodiment 3
By 1 part（g）Initial viscosity-average molecular weight is that the sodium alginate of 38,690,500 dalton is scattered in 50 parts（ml）In 5 mol/L normal propyl alcohol solution, stirring is lower to add 10 parts of the acetic acid solution that molar concentration is 17 mol/Ls（ml）Back flow reaction 0.5 hour at 70 DEG C, reaction system is filtered, filtering residue is washed to neutrality Jing deionized water, 75% ethanol solution, is scattered in 75% ethanol solution, Deca sodium hydroxide solution, conciliation system pH is to more than or equal to 7, by the sodium alginate suspension sucking filtration for obtaining, after filtering residue is Jing 75% washing with alcohol to neutrality, graded ethanol is used（75%th, 95%, dehydrated alcohol）Washing, dehydration.It is vacuum dried at 60 DEG C.Sodium alginate Jing Ubbelohdes viscosimetry after degraded is determined, and viscosity-average molecular weight is 11,633,500 dalton.
Embodiment 4
By 1 part（g）Initial viscosity-average molecular weight is that the sodium alginate of 50,075,000 dalton is scattered in 60 parts（ml）In 18 mol/L ethylene glycol solutions, stirring is lower to add 3 parts of the hydrochloric acid solution that molar concentration is 10 mol/Ls（ml）Back flow reaction 6 hours at 30 DEG C, reaction system is filtered, filtering residue is washed to neutrality Jing deionized water, 75% ethanol solution, is scattered in 75% ethanol solution, Deca sodium hydroxide solution, conciliation system pH is to more than or equal to 7, by the sodium alginate suspension sucking filtration for obtaining, after filtering residue is Jing 75% washing with alcohol to neutrality, graded ethanol is used（75%th, 95%, dehydrated alcohol）Washing, dehydration.It is vacuum dried at 60 DEG C.Sodium alginate Jing Ubbelohdes viscosimetry after degraded is determined, and viscosity-average molecular weight is 11,386,000 dalton.
Claims (4)
1. a kind of biodegrading process of sodium alginate, it is characterised in that sodium alginate is placed in alcohol and acid solution, heterogeneous degraded is carried out in acid condition, by controlling response time and reaction temperature, prepares the sodium alginate of different molecular weight, specially：
1）Sodium alginate is scattered in alcoholic solution, acid solution is added thereto under agitation, the back flow reaction under keeping warm mode, stirring control degradation time, complete degradation reaction；
2）By step 1）The reaction system filtration of gained, deionized water, 75% ethanol are washed till neutrality to solid successively, are then dispersed in 75% ethanol, and stirring is lower to add sodium hydroxide solution, and regulation system pH is to more than or equal to 7；
3）By step 2）The reaction system of gained is filtered, after gained solid is Jing 75% washing with alcohol to neutrality, successively with 75%, 95%, absolute ethanol washing, dehydration, vacuum drying obtains sodium alginate product of degrading.
2. sodium alginate biodegrading process according to claim 1, it is characterised in that step 1）The alcohol for using can be ethanol, ethylene glycol, normal propyl alcohol, isopropanol or methanol, and the concentration of alcoholic solution is 5-24 mol/Ls, and its consumption can be sodium alginate
40-60 times（g/ml）.
3. sodium alginate biodegrading process according to claim 1, it is characterised in that step 1）The acid for being used can be concentrated hydrochloric acid, phosphoric acid or acetic acid, and the concentration of acid solution is 10-17 mol/Ls, and its consumption can be 3-20 times of sodium alginate（g/ml）.
4. sodium alginate biodegrading process according to claim 1, it is characterised in that step 1）Described reflux temperature can be 30-80 DEG C, and the response time can be 0.5-48 hour.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113004434A (en) * | 2021-03-03 | 2021-06-22 | 大连工业大学 | Sodium alginate degradation method based on bismuth tungstate photocatalyst |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103435715A (en) * | 2013-09-02 | 2013-12-11 | 中国科学院烟台海岸带研究所 | Preparation method and application of vanadium complexes of oligosaccharides and derivatives thereof |
| CN103755750A (en) * | 2014-02-10 | 2014-04-30 | 青岛博智汇力生物科技有限公司 | Method for preparing mannuronic acid monosaccharide and guluronic acid monosaccharide |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103435715A (en) * | 2013-09-02 | 2013-12-11 | 中国科学院烟台海岸带研究所 | Preparation method and application of vanadium complexes of oligosaccharides and derivatives thereof |
| CN103755750A (en) * | 2014-02-10 | 2014-04-30 | 青岛博智汇力生物科技有限公司 | Method for preparing mannuronic acid monosaccharide and guluronic acid monosaccharide |
Non-Patent Citations (1)
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| 马成浩 等: "海藻酸钠生产工艺降解情况研究", 《中国食品添加剂》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113004434A (en) * | 2021-03-03 | 2021-06-22 | 大连工业大学 | Sodium alginate degradation method based on bismuth tungstate photocatalyst |
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Application publication date: 20170419 |