CN1321139C - Production process of algin oligose - Google Patents
Production process of algin oligose Download PDFInfo
- Publication number
- CN1321139C CN1321139C CNB200410036382XA CN200410036382A CN1321139C CN 1321139 C CN1321139 C CN 1321139C CN B200410036382X A CNB200410036382X A CN B200410036382XA CN 200410036382 A CN200410036382 A CN 200410036382A CN 1321139 C CN1321139 C CN 1321139C
- Authority
- CN
- China
- Prior art keywords
- algin
- hydrogen peroxide
- oligosaccharide
- algin oligosaccharide
- alginate
- 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
- 235000010443 alginic acid Nutrition 0.000 title claims abstract description 58
- 229920000615 alginic acid Polymers 0.000 title claims abstract description 58
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 18
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 45
- 229920001542 oligosaccharide Polymers 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 239000007800 oxidant agent Substances 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 150000002482 oligosaccharides Chemical class 0.000 claims description 21
- 239000007787 solid Substances 0.000 claims description 13
- 239000007921 spray Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 14
- 239000002994 raw material Substances 0.000 abstract description 5
- 230000001590 oxidative effect Effects 0.000 abstract description 3
- 229940072056 alginate Drugs 0.000 abstract 5
- -1 alginate oligosaccharides Chemical class 0.000 abstract 3
- 239000007790 solid phase Substances 0.000 abstract 3
- FHVDTGUDJYJELY-UHFFFAOYSA-N 6-{[2-carboxy-4,5-dihydroxy-6-(phosphanyloxy)oxan-3-yl]oxy}-4,5-dihydroxy-3-phosphanyloxane-2-carboxylic acid Chemical compound O1C(C(O)=O)C(P)C(O)C(O)C1OC1C(C(O)=O)OC(OP)C(O)C1O FHVDTGUDJYJELY-UHFFFAOYSA-N 0.000 abstract 2
- 238000009776 industrial production Methods 0.000 abstract 1
- 238000005507 spraying Methods 0.000 abstract 1
- 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 description 5
- 229960001126 alginic acid Drugs 0.000 description 5
- 239000000783 alginic acid Substances 0.000 description 5
- 150000004781 alginic acids Chemical class 0.000 description 5
- 239000004615 ingredient Substances 0.000 description 5
- 239000000661 sodium alginate Substances 0.000 description 5
- 235000010413 sodium alginate Nutrition 0.000 description 5
- 229940005550 sodium alginate Drugs 0.000 description 5
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 239000011591 potassium Substances 0.000 description 3
- 229910052700 potassium Inorganic materials 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229920000856 Amylose Polymers 0.000 description 1
- 241000512259 Ascophyllum nodosum Species 0.000 description 1
- 241000227647 Fucus vesiculosus Species 0.000 description 1
- 241000199919 Phaeophyceae Species 0.000 description 1
- 229920000297 Rayon Polymers 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000010525 oxidative degradation reaction Methods 0.000 description 1
- 235000011837 pasties Nutrition 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
Landscapes
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention provides a production process of alginate oligosaccharides, which comprises the following sequential steps of (1) uniformly spraying hydrogen peroxide serving as an oxidant on solid-phase alginate with the water content of 10-85% by weight, fully mixing the solid-phase alginate and the oxidant in a weight ratio of 100: 1-10, and continuously stirring at the temperature of 50-90 ℃ to obtain the alginate oligosaccharides with the viscosity value of 1-20 cps. (2) Removing residual hydrogen peroxide from alginate oligosaccharide and drying; the step (2) is as follows: vacuumizing the algin oligose to remove residual hydrogen peroxide and partial water until the water content of the material is less than 50%, and drying the material in a dryer. The process degrades the raw material algin in a solid phase system, has simple production process and high product yield, and is suitable for industrial production.
Description
Technical field
The present invention relates to the production technique of a kind of ultra-low molecular amount alginic acid and salt thereof, i.e. the production technique of algin oligosaccharide.
Background technology
Algin is the general designation of alginic acid and salt (as sodium alginate, Potassium polyalginate etc.) thereof, is a kind of natural macromolecule amylose polymkeric substance that extracts from phaeophyta marine plants such as sea-tangle, bulk kelp, bladder wrack, sargassun.Algin is widely used in medicine, food, chemical industry, agriculture field as raw material, studies show that algin has more activity when lower molecular weight.Existing algin oligosaccharide adopts to degrade in liquid-phase system usually and obtains, be about to raw material algin product and add a certain amount of water and ethanol, adding oxygenant then under liquid phase stirs, until the low viscosity algin that needing to obtain viscosity, as Chinese patent 99316981 disclosed technical schemes.The shortcoming of above-mentioned technology is, prepares low viscosity algin in liquid phase, when reach need viscosity after, algin suspension changes pasty state into, and is unsuitable dry, after centrifugation, low-molecular-weight algal glue runs off in preparation process seriously, and yield only is about 50% of a material quantity.
Summary of the invention
The present invention has overcome the deficiency that existing production algin oligosaccharide exists, a kind of production technique of simple and effective algin oligosaccharide is provided, under solid system the raw material algin has been degraded, this production technique is simple, product yield height is suitable for suitability for industrialized production.
For realizing goal of the invention of the present invention, the present invention adopts following technical proposals.
The production technique that the invention discloses a kind of algin oligosaccharide comprises the following order step,
(1) be evenly to spray oxidants hydrogen peroxide on the solid state shape algin of 10-85% at weight in wet base per-cent, the weight ratio of solid state shape algin and oxygenant is 100: 1～10, thorough mixing, under 50-90 ℃ of temperature control condition, continuously stirring obtains the algin oligosaccharide of viscosity number at 1-20cps.
The production technique of described algin oligosaccharide further comprises the following steps:
(2) algin oligosaccharide is dispeled residual hydrogen peroxide and carry out drying;
Described step (2) is: algin oligosaccharide is vacuumized dispel residual hydrogen peroxide and part moisture, less than 50% o'clock, material is delivered to the moisture eliminator drying until material moisture.
The solid state shape algin be weight in wet base per-cent be 10-85% between the algin solid.
H
2O
2Can select the superoxol of commercially available common concentration, concentration is selected weight percent 27.5%, 30% etc. usually, adjusts extremely above-mentioned ratio of algin and hydrogen peroxide by suitable proportioning.
Above-mentioned whipping process can be any mode that mixes of prior art, and mixing frequency can regulate according to the viscosity index of mixture, and churning time is regulated according to the difference of mixture concentration, needing to obtain the algin oligosaccharide of viscosity.Common churning time is: 5-25 hour.
In the technique scheme, add oxidants hydrogen peroxide in the algin raw material, hydrogen peroxide has than strong oxidizing property, and it can become the low viscous algin of lower molecular weight, i.e. algin oligosaccharide by oxidative degradation with the full-bodied algin of high molecular.Owing in solid system, carry out DeR, by regularly measuring algin viscosity, after reaching the viscosity number that needs (selecting Wu Shi viscosity characteristics viscosity number usually between 1～20), it is Powdered uniformly that material is, directly carry out drying treatment, just can obtain required algin oligosaccharide product.
The production technique of above-mentioned algin oligosaccharide, because the manufacturing processed moisture content of material is few, so drying process is simple, cost reduces, further, because in preparation process, algin is loss not, so product yield height.
Embodiment
Embodiment 1
Get 100 kilograms of water content and be 85% solid state shape brown alga blob of viscose, evenly spray and add 13 kilograms and contain effective ingredient (H
2O
2) weight percent concentration is 30% hydrogen peroxide, thorough mixing places 60 ℃ of sealed can temperature controls, heating was also stirred 20 hours, opened vacuum unit transpiring moisture and hydrogen peroxide, reduced to 49.5% to water content, emit material and carry out drying, the alginic acid product that obtains, viscosity is 3cps.
Embodiment 2
Get 100 kilograms of water content and be 10% solid state shape algin sodium alginate, evenly spray and add 30 kilograms to contain effective ingredient be 27.5% hydrogen peroxide, thorough mixing, place 90 ℃ of sealed can temperature controls, heat and stirred 5 hours, open vacuum unit transpiring moisture and hydrogen peroxide, reduce to 40% to water content, emit material and carry out drying, the sodium alginate product that obtains, viscosity is 5cps.
Embodiment 3
Get 100 kilograms of water content and be 30% solid state shape algin Potassium polyalginate, evenly spray and add 3.4 kilograms to contain effective ingredient be 30% hydrogen peroxide, thorough mixing, place 50 ℃ of sealed can temperature controls, heat and stirred 15 hours, open vacuum unit transpiring moisture and hydrogen peroxide, reduce to 28% to water content, emit material and carry out drying, the Potassium polyalginate product that obtains, viscosity is 2cps.
Embodiment 4
Get 100 kilograms of water content and be 35% solid state shape algin alginic acid, evenly spray and add 36 kilograms to contain effective ingredient be 27.5% hydrogen peroxide, thorough mixing, place 70 ℃ of sealed can temperature controls, heat and stirred 20 hours, open vacuum unit transpiring moisture and hydrogen peroxide, reduce to 35% to water content, emit material and carry out drying, the alginic acid product that obtains, viscosity is 5cps.
Embodiment 5
Get 100 kilograms of water content and be 70% solid state shape algin sodium alginate, evenly spray and add 30 kilograms to contain effective ingredient be 27.5% hydrogen peroxide, thorough mixing, place 80 ℃ of sealed can temperature controls, heat and stirred 25 hours, open vacuum unit transpiring moisture and hydrogen peroxide, reduce to 25% to water content, emit material and carry out drying, the sodium alginate product that obtains, viscosity is 3.5cps.
Claims (3)
1, a kind of production technique of algin oligosaccharide comprises the following order step,
(1) be evenly to spray oxidants hydrogen peroxide on the solid state shape algin of 10-85% at weight in wet base per-cent, the weight ratio of solid state shape algin and oxygenant is 100: 1～10, thorough mixing, under 50-90 ℃ of temperature control condition, continuously stirring obtains the algin oligosaccharide of viscosity number at 1-20cps.
2, the production technique of algin oligosaccharide according to claim 1 is characterized in that,
The production technique of described algin oligosaccharide further comprises the following steps:
(2) algin oligosaccharide is dispeled residual hydrogen peroxide and carry out drying.
3, the production technique of algin oligosaccharide according to claim 2 is characterized in that,
Described step (2) is: algin oligosaccharide is vacuumized dispel residual hydrogen peroxide and part moisture, less than 50% o'clock, material is delivered to the moisture eliminator drying until material moisture.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200410036382XA CN1321139C (en) | 2004-11-22 | 2004-11-22 | Production process of algin oligose |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200410036382XA CN1321139C (en) | 2004-11-22 | 2004-11-22 | Production process of algin oligose |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1631905A CN1631905A (en) | 2005-06-29 |
| CN1321139C true CN1321139C (en) | 2007-06-13 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB200410036382XA Expired - Fee Related CN1321139C (en) | 2004-11-22 | 2004-11-22 | Production process of algin oligose |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1321139C (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101168570B (en) * | 2007-11-15 | 2010-05-26 | 暨南大学 | Method for degrading kelp polysaccharide sulfate |
| CN102370655B (en) * | 2010-08-24 | 2012-12-12 | 青岛大学 | Application of alginate oligosaccharide to preparation of medicament for facilitating postnatal uterine contraction |
| CN102492053B (en) * | 2011-12-28 | 2013-04-17 | 青岛明月海洋科技有限公司 | Preparation method of high-viscosity alginate |
| CN103665183A (en) * | 2013-12-18 | 2014-03-26 | 青岛福创环境科技有限公司 | Producing method of sodium alginate with ultralow viscosity |
| CN105315384A (en) * | 2014-06-18 | 2016-02-10 | 山东大学（威海） | Method of producing alginate-derived oligosaccharide through gradient dilution and oxidization |
| CN112442138A (en) * | 2020-11-26 | 2021-03-05 | 青岛聚大洋藻业集团有限公司 | Preparation method of high-purity sodium alginate and application of high-purity sodium alginate in biological 3D printing |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60186503A (en) * | 1984-03-06 | 1985-09-24 | Fuji Kagaku Kogyo Kk | Preparation of high polymer consisting essentially of alginate |
| CN1380342A (en) * | 2001-04-07 | 2002-11-20 | 青岛海洋大学 | Production method of phycocolloid oligosaccharide |
| CN1414002A (en) * | 2002-09-20 | 2003-04-30 | 青岛海洋大学 | Method for preparing algin oligose using chemical oxidation |
-
2004
- 2004-11-22 CN CNB200410036382XA patent/CN1321139C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60186503A (en) * | 1984-03-06 | 1985-09-24 | Fuji Kagaku Kogyo Kk | Preparation of high polymer consisting essentially of alginate |
| CN1380342A (en) * | 2001-04-07 | 2002-11-20 | 青岛海洋大学 | Production method of phycocolloid oligosaccharide |
| CN1414002A (en) * | 2002-09-20 | 2003-04-30 | 青岛海洋大学 | Method for preparing algin oligose using chemical oxidation |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1631905A (en) | 2005-06-29 |
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Application publication date: 20050629 Assignee: JIANGSU MINGYUE MARINE BIOTECHNOLOGY Co.,Ltd. Assignor: QINGDAO BRIGHT MOON SEAWEED Group Contract record no.: 2013370000253 Denomination of invention: Algin oligosaccharide preparing method Granted publication date: 20070613 License type: Exclusive License Record date: 20131205 |
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| LICC | Enforcement, change and cancellation of record of contracts on the licence for exploitation of a patent or utility model | ||
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Granted publication date: 20070613 |