CN101942121B - Method for improving viscosity and stability of sodium alga acid - Google Patents
Method for improving viscosity and stability of sodium alga acid Download PDFInfo
- Publication number
- CN101942121B CN101942121B CN201010503992A CN201010503992A CN101942121B CN 101942121 B CN101942121 B CN 101942121B CN 201010503992 A CN201010503992 A CN 201010503992A CN 201010503992 A CN201010503992 A CN 201010503992A CN 101942121 B CN101942121 B CN 101942121B
- Authority
- CN
- China
- Prior art keywords
- solution
- sodium alginate
- viscosity
- stability
- sodium alga
- 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.)
- Expired - Fee Related
Links
- 238000000034 method Methods 0.000 title claims abstract description 18
- 239000002253 acid Substances 0.000 title claims abstract description 13
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 title abstract 10
- 229910052708 sodium Inorganic materials 0.000 title abstract 10
- 239000011734 sodium Substances 0.000 title abstract 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 238000000108 ultra-filtration Methods 0.000 claims abstract description 12
- 229920002582 Polyethylene Glycol 600 Polymers 0.000 claims abstract description 8
- 230000001105 regulatory effect Effects 0.000 claims abstract description 6
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 70
- 235000010413 sodium alginate Nutrition 0.000 claims description 69
- 229940005550 sodium alginate Drugs 0.000 claims description 69
- 239000000661 sodium alginate Substances 0.000 claims description 69
- 239000000243 solution Substances 0.000 claims description 32
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- FPQQSJJWHUJYPU-UHFFFAOYSA-N 3-(dimethylamino)propyliminomethylidene-ethylazanium;chloride Chemical compound Cl.CCN=C=NCCCN(C)C FPQQSJJWHUJYPU-UHFFFAOYSA-N 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 5
- 230000004913 activation Effects 0.000 claims description 5
- 239000012670 alkaline solution Substances 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 2
- 239000001117 sulphuric acid Substances 0.000 claims description 2
- 235000011149 sulphuric acid Nutrition 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 6
- 239000012535 impurity Substances 0.000 abstract description 5
- 239000003814 drug Substances 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 3
- 239000012876 carrier material Substances 0.000 abstract description 2
- 230000008014 freezing Effects 0.000 abstract 2
- 238000007710 freezing Methods 0.000 abstract 2
- 230000003213 activating effect Effects 0.000 abstract 1
- 239000012141 concentrate Substances 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 238000003756 stirring Methods 0.000 abstract 1
- 238000013268 sustained release Methods 0.000 abstract 1
- 239000012730 sustained-release form Substances 0.000 abstract 1
- 239000004753 textile Substances 0.000 abstract 1
- 238000005303 weighing Methods 0.000 description 9
- 230000008859 change Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000013019 agitation Methods 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 230000001143 conditioned effect Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000004132 cross linking Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 241000270666 Testudines Species 0.000 description 1
- 235000010443 alginic acid Nutrition 0.000 description 1
- 229920000615 alginic acid Polymers 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 231100000957 no side effect Toxicity 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
Landscapes
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention discloses a method for improving viscosity and stability of sodium alga acid, which comprises the following steps of: (1) preparing solution of sodium alga acid; (2) regulating the pH value of the solution of sodium alga acid to be 4.0-6.0 by using acid, and fully stirring the solution; (3) adding EDC.HCl into the solution of sodium alga acid, and activating the sodium alga acid at room temperature; (4) taking solution of PEG600, and adding into the solution of sodium alga acid for reaction; (5) regulating the pH value of the reaction solution to be 7.0 by using base solution, and terminating the reaction; (6) performing ultrafiltration on the reacted solution by using a film so as to remove small molecular impurities therein and concentrate; and (7) completing the ultrafiltration, pre-freezing the solution for 10 to 14 hours, and freezing and drying so as to prepare high-viscosity high-stability sodium alga acid. The method has the advantages of capacity of obviously improving viscosity and stability of the sodium alga acid, simple and easily controlled technology, readily available raw materials, low cost, and easy popularization and application. The prepared high-viscosity high-stability sodium alga acid can be used for degradable gelatinous materials, medicament sustained-release materials, biological carrier materials, tissue engineering materials and other medicinal purposes, and also can be applied to the food industry, printing and textile industry and the like.
Description
Technical field
The present invention relates to a kind of method that improves sodium alginate viscosity and stability, belong to biological chemical field.
Background technology
As everyone knows, sodium alginate is as a kind of natural high molecular substance, with its favorable biological degradability and biocompatibility, and good thickening, film-forming properties, stability, flocculence and closing property of huge legendary turtle and be widely used in fields such as chemistry, biology, medicine, food.Along with the sodium alginate application and development, market is more and more higher with the requirement of stability to the quality of sodium alginate.
But the outstanding problem of current existence is: no matter in the aqueous solution or contain in the dry product of a certain amount of moisture, degraded in various degree all can take place in sodium alginate, causes the reduction of sodium alginate product viscosity.This phenomenon brings many difficulties for production, storage and the application of alginates product.In Industrial processes, sodium alginate extraction process point is various, has signs of degradation and causes product yield low, and viscosity is not high.Because effective control degradation, quality product is difficult to stablize.In storage and application process, degraded in various degree also can take place in sodium alginate, and its sign is the continuous decline of viscosity, and the distribution range of its average molecular mass and relative molecular mass also can constantly change.
Since last century the seventies, the traditional extraction technique of sodium alginate is not realized fundamental change, and processing step is numerous and diverse, degraded is serious.The mechanism of degraded is still indeterminate at present, and concrete mechanism remains further to be studied.Sex change research to sodium alginate in the prior art does not all have substantial breakthrough, its modified product all not to have to carry out industrialization.Because the singularity of sodium alginate structure does not also have a kind of effective means to come the generation of complete control degradation at present.
Summary of the invention
At above-mentioned prior art, at sodium alginate instability, degradation-labile defect, the invention provides a kind of method that improves sodium alginate viscosity and stability, it be a kind ofly have no side effect, the method for low-cost, simple to operate crosslinked sodium alginate, and, realize improving the purpose of sodium alginate viscosity and stability by control to reaction conditions.
The present invention is achieved by the following technical solutions:
A kind of method that improves sodium alginate viscosity and stability, its step is as follows:
(1) sodium alginate is joined in the deionized water, compound concentration is 0.1～0.5% (w/v, sodium alginate soln g/L);
(2) with sour pH value to 4.0～6.0 of regulating sodium alginate soln, and abundant stirred solution;
(3) EDCHCl is joined in the sodium alginate soln activation sodium alginate 0.5～1.5h under the room temperature;
(4) get the PEG600 solution that concentration is 0.01～0.05g/ml, join in the sodium alginate soln, reaction 1～3h;
(5) regulate the pH value to 7.0 of above-mentioned reaction soln with alkaline solution, termination reaction;
(6) be that 10000 film carries out ultrafiltration with above-mentioned reacted solution molecular weight cut-off, removing small molecular weight impurity wherein, and play spissated effect;
(7) after the ultrafiltration fully, solution is carried out pre-freeze 10～14h, carry out lyophilize then, promptly obtain the sodium alginate of high viscosity and high stability.
In the described step (2), the acid of regulating pH is hydrochloric acid or sulphuric acid soln.
In the described step (3), EDC is 1-ethyl-3-[3-(dimethyl amido) propyl group]-carbodiimide, EDCHCl is the title complex that EDC and HCl form, and is commercialization product form.
In the described step (3), the molar percentage of EDC and sugar unit is 1～3%.
In the described step (4), the mol ratio of PEG600 and EDC is 1: (2～3).
In the described step (5), alkaline solution is a sodium hydroxide solution.
Handle the sodium alginate that obtains through aforesaid method, after testing, sodium alginate viscosity improves 8.5%～15%, and thermostability also increases.
Adopt method of the present invention to handle sodium alginate, can obviously improve its viscosity and stability, technology of the present invention is simple and easy to control, starting material are easy to get, cost is low, be easy to apply, high viscosity for preparing and high stability sodium alginate product can be used for medical usages such as degradable gel material, medicament slow release material, bio-carrier material, tissue engineering material, also can be used for foodstuffs industry and seal spins industry etc.
Embodiment
The present invention is further illustrated below in conjunction with embodiment.
1 one kinds of methods that improve sodium alginate viscosity and stability of embodiment
Step is as follows:
(1) take by weighing the 5g sodium alginate and join in the 1L deionized water, magnetic agitation is dissolved fully until sodium alginate, obtains 0.5% (w/v) sodium alginate soln.
(2) regulate the pH value to 4.0 of above-mentioned sodium alginate soln with 0.1mol/LHCl solution, fully stirred solution.
(3) take by weighing EDCHCl 0.049g, join in the above-mentioned sodium alginate soln, activation sodium alginate 1h under the room temperature.
(4) take by weighing PEG6000.077g,, PEG600 solution is joined react 2h in the sodium alginate soln then with deionized water 3ml dissolving.
(5) the pH value to 7.0 of usefulness 0.1mol/LNaOH solution conditioned reaction solution, termination reaction.
(6) be that 10000 film carries out ultrafiltration with above-mentioned reacted solution molecular weight cut-off, remove small molecular weight impurity wherein, and play spissated effect.
(7) after the ultrafiltration fully solution is carried out pre-freeze 12h, carry out lyophilize then, finally obtain high viscosity and high stability sodium alginate product.Detect sodium alginate viscosity raising 15.0% through Ubbelohde viscometer and rotational viscosimeter; (w/v, g/L) sodium alginate cross-linking product place water-bath to change with the viscosity of rotary viscosity design determining solution from 20 ℃ to 70 ℃ solution, and the result shows that sodium alginate cross-linking product thermostability improves in preparation 0.5%.
2 one kinds of methods that improve sodium alginate viscosity and stability of embodiment
Step is as follows:
(1) take by weighing the 5g sodium alginate and join in the 1L deionized water, magnetic agitation is dissolved fully until sodium alginate, obtains 0.5% (w/v) sodium alginate soln.
(2) with the pH value to 5.0 of 0.1mol/LHCl solution adjusting sodium alginate soln, abundant stirred solution.
(3) take by weighing EDCHCl 0.025g, join in the sodium alginate soln, activation sodium alginate 1h under the room temperature.
(4) take by weighing PEG6000.038g,, PEG600 solution is joined react 2h in the sodium alginate soln then with deionized water 3ml dissolving.
(5) the pH value to 7.0 of usefulness 0.1mol/LNaOH solution conditioned reaction solution, termination reaction.
(6) be that 10000 film carries out ultrafiltration with the reaction soln molecular weight cut-off, remove small molecular weight impurity wherein, and play spissated effect.
(7) after the ultrafiltration fully solution is carried out pre-freeze 12h, carry out lyophilize then, finally obtain high viscosity and high stability sodium alginate product.Sodium alginate viscosity improves 8.5% after testing, and thermostability also increases.
3 one kinds of methods that improve sodium alginate viscosity and stability of embodiment
Step is as follows:
(1) take by weighing the 5g sodium alginate and join in the 1L deionized water, magnetic agitation is dissolved fully until sodium alginate, obtains 0.5% (w/v) sodium alginate soln.
(2) with the pH value to 5.0 of 0.1mol/LHCl solution adjusting sodium alginate soln, abundant stirred solution.
(3) take by weighing EDCHCl 0.073g, join in the sodium alginate soln, activation sodium alginate 0.5h under the room temperature.
(4) take by weighing PEG6000.115g,, PEG600 solution is joined react 2h in the sodium alginate soln then with deionized water 3ml dissolving.
(5) the pH value to 7.0 of usefulness 0.1mol/LNaOH solution conditioned reaction solution, termination reaction.
(6) be that 10000 film carries out ultrafiltration with the reaction soln molecular weight cut-off, remove small molecular weight impurity wherein, and play spissated effect.
(7) after the ultrafiltration fully solution is carried out pre-freeze 12h, carry out lyophilize then, finally obtain high viscosity and high stability sodium alginate product.Sodium alginate viscosity improves 10.5% after testing, and thermostability also increases.
Claims (3)
1. one kind is improved sodium alginate viscosity and stable method, it is characterized in that its step is as follows:
(1) sodium alginate is joined in the deionized water, compound concentration is 0.1～0.5% sodium alginate soln;
(2) with sour pH value to 4.0～6.0 of regulating sodium alginate soln, and abundant stirred solution;
(3) EDCHCl is joined in the sodium alginate soln activation sodium alginate 0.5～1.5h under the room temperature;
(4) get the PEG600 solution that concentration is 0.01～0.05g/ml, join in the sodium alginate soln, reaction 1～3h;
(5) regulate the pH value to 7.0 of above-mentioned reaction soln with alkaline solution, termination reaction;
(6) be that 10000 film carries out ultrafiltration with above-mentioned reacted solution molecular weight cut-off;
(7) after the ultrafiltration fully, solution is carried out pre-freeze 10～14h, carry out lyophilize then, promptly obtain the sodium alginate of high viscosity and high stability;
Described EDC is 1-ethyl-3-[3-(dimethyl amido) propyl group]-carbodiimide;
In the described step (3), the molar percentage of EDC and sugar unit is 1～3%;
In the described step (4), the mol ratio of PEG600 and EDC is 1: (2～3).
2. a kind of method that improves sodium alginate viscosity and stability according to claim 1, it is characterized in that: in the described step (2), the acid of regulating pH is hydrochloric acid or sulphuric acid soln.
3. a kind of method that improves sodium alginate viscosity and stability according to claim 1, it is characterized in that: in the described step (5), alkaline solution is a sodium hydroxide solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010503992A CN101942121B (en) | 2010-10-12 | 2010-10-12 | Method for improving viscosity and stability of sodium alga acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010503992A CN101942121B (en) | 2010-10-12 | 2010-10-12 | Method for improving viscosity and stability of sodium alga acid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101942121A CN101942121A (en) | 2011-01-12 |
| CN101942121B true CN101942121B (en) | 2011-12-14 |
Family
ID=43434339
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201010503992A Expired - Fee Related CN101942121B (en) | 2010-10-12 | 2010-10-12 | Method for improving viscosity and stability of sodium alga acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101942121B (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103130912B (en) * | 2011-12-02 | 2015-08-12 | 江南大学 | Single stage method prepares covalent cross-linking and hydrophobically modified Sodium Alginate Hydrogel Films |
| CN102603918B (en) * | 2012-03-16 | 2013-11-06 | 扬州大学 | Preparation method of beta-cyclodextrin-grafted alginic acid derivative |
| CN105330875B (en) * | 2015-11-23 | 2019-01-29 | 青岛大学 | A kind of cross-linking modified sodium alginate and preparation method thereof |
| CN111333749A (en) * | 2020-03-27 | 2020-06-26 | 广州古泉生物科技有限公司 | Preparation and application of polypropylene oxide-sodium alginate hydrogel |
| CN113774686B (en) * | 2021-09-17 | 2023-07-11 | 绍兴永通印花有限公司 | Reactive printing paste and rotary screen printing application thereof |
| CN117089543B (en) * | 2023-10-19 | 2024-02-27 | 杭州尚善若水环保科技有限公司 | Water treatment microbial inoculum and application thereof in aquaculture wastewater treatment |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6749865B2 (en) * | 2000-02-15 | 2004-06-15 | Genzyme Corporation | Modification of biopolymers for improved drug delivery |
| CN101260160A (en) * | 2008-04-23 | 2008-09-10 | 海南大学 | A kind of method of partially oxidizing sodium alginate |
| CN101831002B (en) * | 2009-03-11 | 2011-11-16 | 中国科学院大连化学物理研究所 | Preparation method of sodium alginate for tissue engineering |
-
2010
- 2010-10-12 CN CN201010503992A patent/CN101942121B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN101942121A (en) | 2011-01-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101942121B (en) | Method for improving viscosity and stability of sodium alga acid | |
| CN101613893B (en) | Bacterial cellulose/sodium alginate composite fiber and preparation method thereof | |
| CN105622780B (en) | A kind of homogeneous preparation method of quaternized chitin | |
| CN108727610B (en) | Double-network hydrogel with high toughness, shape memory and self-repairing characteristics and preparation method thereof | |
| CN106496639A (en) | A kind of nano-cellulose polypyrrole polyvinyl alcohol composite conducting hydrogel and its preparation method and application | |
| CN101260160A (en) | A kind of method of partially oxidizing sodium alginate | |
| CN103087334B (en) | Method for preparing composite hydrogel of sodium alginate and artemisia desertorum seed gum | |
| CN106467613A (en) | A kind of self-healing polyanion-chitin quarternary ammonium salt aquagel and its application | |
| CN104262648B (en) | It is a kind of using dialdehyde polyethylene glycol as collagen base biological medical material of crosslinking agent and preparation method thereof | |
| CN105079886A (en) | Preparation method of oxidized nano-cellulose/collagen composite sponge | |
| CN103788217A (en) | Cellulose gel material, preparation method and applications | |
| CN107141519B (en) | A modified chitosan-based superabsorbent hydrogel and its preparation and application | |
| CN102605467A (en) | Method for preparing composite polyelectrolyte fiber membrane by utilizing freeze-drying way | |
| CN110694594A (en) | Preparation method of porous materials based on graphene oxide, chitosan and dopamine | |
| CN103834045A (en) | Two-way reversible temperature-sensitive gel and preparation method and application thereof | |
| CN100391981C (en) | A kind of preparation method of completely water-soluble low molecular weight chitosan/chitooligosaccharide | |
| CN106519060A (en) | Preparation of carboxymethyl curdlan | |
| CN102634040B (en) | Basic solvent for dissolving chitosan and method for dissolving chitosan under alkaline condition | |
| CN112773942B (en) | A kind of preparation method of injectable self-healing antibacterial hydrogel | |
| CN107200853B (en) | A kind of dendrimer/carboxymethyl cellulose superabsorbent gel and its preparation and application | |
| CN101724095A (en) | Preparation method of carboxymethyl chitosan quaternary ammonium salt in water phase by microwave radiation | |
| JP2010106068A (en) | New chemical modification method for polysaccharide | |
| CN102120823B (en) | The synthesis of water solublity zein and the utilization in pharmaceutical preparation | |
| CN107987181A (en) | A kind of preparation method and application of hydroxypropyl curdlan | |
| CN106497050A (en) | With rosin acid as template and the dopant method for preparing Preparation of conductive polyaniline nanotubes |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20111214 Termination date: 20141012 |
|
| EXPY | Termination of patent right or utility model |