CN105754009A - Production process of super-low-viscosity magnesium alginate - Google Patents
Production process of super-low-viscosity magnesium alginate Download PDFInfo
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- CN105754009A CN105754009A CN201511024283.4A CN201511024283A CN105754009A CN 105754009 A CN105754009 A CN 105754009A CN 201511024283 A CN201511024283 A CN 201511024283A CN 105754009 A CN105754009 A CN 105754009A
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- alginic acid
- acid magnesium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/006—Heteroglycans, i.e. polysaccharides having more than one sugar residue in the main chain in either alternating or less regular sequence; Gellans; Succinoglycans; Arabinogalactans; Tragacanth or gum tragacanth or traganth from Astragalus; Gum Karaya from Sterculia urens; Gum Ghatti from Anogeissus latifolia; Derivatives thereof
- C08B37/0084—Guluromannuronans, e.g. alginic acid, i.e. D-mannuronic acid and D-guluronic acid units linked with alternating alpha- and beta-1,4-glycosidic bonds; Derivatives thereof, e.g. alginates
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Abstract
The invention discloses a production process of super-low-viscosity magnesium alginate.The production process is characterized by including following steps: (1), cleaning and chopping brown alga, adding water of five times and 15% composite magnesium salt, and disposing in a high-temperature high-pressure reaction kettle for degradation for 50-60 min; (2), roughly filtering to obtain magnesium alginate rough extract; (3), adding activated carbon into the magnesium alginate rough extract for adsorption and decoloring, and filtering to obtain primarily-purified extract; (4), performing further purifying and impurity removing on the primarily-purified extract through ion exchange resin adsorption to obtain purified extract; (5), concentrating the purified extract; (6), spray-drying concentrate to obtain solid powder of magnesium alginate.Rotary viscosity of 1% glue liquid of magnesium alginate prepared by the production process at 20 DEG C is 5-10 mPa.s.
Description
Technical field
The present invention relates to the production technology of a kind of ultra-low viscosity alginic acid magnesium.
Background technology
Alginic acid magnesium is the alginate of monovalence, is the macromolecular polysaccharide class material extracted from the Brown algae plants such as Thallus Laminariae (Thallus Eckloniae), has the good characteristics such as natural, green, biocompatibility is high, and the alginate product that the characteristic of product is also known from other has bigger different.Ultra-low viscosity alginic acid magnesium is only bivalence not gel alginate, there is the feature of easily absorption, the effect reducing blood fat can be played, as the main composition of health food or health-nutrition food or dispensing, can regulate and prophylaxis of hypertension, retarding cardiovascular is old and feeble, improve microcirculation.
Domestic at present rarely have enterprise to produce ultra-low molecular alginic acid magnesium, and the production technology of this product is immature, and the production technology of conventional alginic acid magnesium, the production cycle is long, is not easily absorbed by organisms when product viscosity height, poor quality, practical application.
For prior art present situation, we are by High Temperature High Pressure degraded raw material Brown algae technology, solution production cycle length, the shortcoming that product viscosity is high；Employing compound magnesium salt carries out digesting neutralization reaction, and solution traditional production technique existence neutralization is reacted not exclusively, the response time is long, the inhomogenous drawback of finished product；Advanced ion exchange resin exchange adsorption technology is adopted to be greatly improved the quality of product.
Summary of the invention
The present invention is directed to above-mentioned technical barrier and invented " production technology of a kind of ultra-low viscosity alginic acid magnesium ".The present invention adopts high-temperature high-pressure reaction kettle technology directly to degrade raw material Brown algae, solves traditional processing technology cycle length, drawback that product viscosity is high, and the water consumption simultaneously significantly solved is both economically and environmentally beneficial.Additionally, the present invention adopts compound magnesium salt to carry out digesting neutralization reaction, solution traditional production technique existence neutralization is reacted not exclusively, the response time is long, the inhomogenous drawback of finished product.
In order to realize foregoing invention purpose, the present invention adopts following technical proposals to be achieved:
The production technology of a kind of alginic acid magnesium, said method comprising the steps of:
(1) water and the 15% compound magnesium salt of 5 times is cleaned, shredded, adds to Brown algae, is placed in degradation treatment in high temperature, autoclave, processes time 50-60min；
(2) coarse filtration obtains alginic acid magnesium crude extract；
(3) in alginic acid magnesium crude extract, add activated carbon adsorption decolouring, filter, it is thus achieved that the extracting solution just purified；
(4) extracting solution of preliminary purification is by ion exchange resin absorption purification further, roguing, obtains the extracting solution of purification；
(5) the extracting solution concentration of purification；
(6) concentrated solution carries out spray drying, obtains the pressed powder of alginic acid magnesium.
Technical scheme is improved further: in described step (1), Brown algae mainly includes Thallus Laminariae (Thallus Eckloniae), Macrocystis pyrifera (L.) Ag., Alga Sgrgassi Enerves.
Technical scheme is improved further: in described step (1) treatment temperature be 250 300 DEG C, processing pressure be 200 300MPa..
Technical scheme is improved further: in described step (1), compound magnesium salt is one or more in magnesium bicarbonate, magnesium hydroxide, magnesium carbonate.
Technical scheme is improved further: described step (4) ion exchange resin is cation exchange resin.
Technical scheme being improved further: in described step (5), adopt vacuum-concentrcted, vacuum is 0.06 0.08MPa, and concentration-temperature is 80-100 DEG C, and concentration time is 20 25min.
Technical scheme being improved further: in described step (5), the temperature of spray drying is 60-75 DEG C, drying time is 1 1.5h.
Compared with prior art, advantages of the present invention and having the benefit effect that
1, high-temperature high-pressure reaction kettle technology degraded raw material alginic acid, the production cycle being greatly shortened, the water consumption simultaneously significantly solved, both economically and environmentally beneficial.
2, compound magnesium salt makes to neutralize and reacts homogeneous, complete, rapid, has ensured homogeneity and the stability of product.
3, advanced ion exchange resin exchange adsorption technology is adopted to be greatly improved the quality of product.
4, the rotary viscosity under the 20 DEG C of conditions of 1% glue of the alginic acid magnesium that the present invention produces is 5 10mPa.s, and it is played positive impetus in the application of health care, field of medicaments by this.
Specific embodiment
Embodiment 1
1, preparation technology
(1) take without rotten Thallus Laminariae (Thallus Eckloniae) 100kg, rinse well with water, Thallus Laminariae (Thallus Eckloniae) is cut into 10 15cm strips, it is placed in autoclave, the water of 500L volume is added in reactor, add 75kg magnesium bicarbonate, reactor parameter, reaction temperature 250 DEG C are set, reactor pressure 200MPa, reacts 50min；
(2) reaction terminates rear coarse filtration and obtains alginic acid magnesium crude extract；
(3) in alginic acid magnesium crude extract, add activated carbon adsorption decolouring, filter, it is thus achieved that the extracting solution just purified；
(4) extracting solution of preliminary purification by cationic exchange resin adsorption purify further, roguing, obtain the extracting solution of purification；
(5) adopting vacuum-concentrcted method, the extracting solution concentration to purification, parameter is vacuum 0.08MPa, temperature 100 DEG C, and concentration time is 20min.
(6) concentrated solution carries out spray drying, and the temperature of spray drying is 60 DEG C, and drying time is 1.5h, obtains the pressed powder of alginic acid magnesium.
2, product viscosity index
Rotary viscosity under 20 DEG C of conditions of 1% glue of alginic acid magnesium prepared by said method is 10mPa.s.
Embodiment 2
1, preparation technology
(1) take without rotten Macrocystis pyrifera (L.) Ag. 100kg, rinse well with water, Thallus Laminariae (Thallus Eckloniae) is cut into 10 15cm strips, it is placed in autoclave, the water of 500L volume is added in reactor, add 35kg magnesium bicarbonate, 20kg hydroxide and 20kg magnesium magnesium carbonate, reactor parameter, reaction temperature 300 DEG C are set, reactor pressure 300MPa, reacts 60min；
(2) reaction terminates rear coarse filtration and obtains alginic acid magnesium crude extract；
(3) in alginic acid magnesium crude extract, add activated carbon adsorption decolouring, filter, it is thus achieved that the extracting solution just purified；
(4) extracting solution of preliminary purification by cationic exchange resin adsorption purify further, roguing, obtain the extracting solution of purification；
(5) adopting vacuum-concentrcted method, the extracting solution concentration to purification, parameter is vacuum 0.07MPa, temperature 80 DEG C, and concentration time is 25min.
(6) concentrated solution carries out spray drying, and the temperature of spray drying is 75 DEG C, and drying time is the 1h pressed powder obtaining alginic acid magnesium.
2, product viscosity index
Rotary viscosity under 20 DEG C of conditions of 1% glue of alginic acid magnesium prepared by said method is 5mPa.s.
Embodiment 3
1, preparation technology
(1) take without rotten Alga Sgrgassi Enerves 100kg, rinse well with water, Thallus Laminariae (Thallus Eckloniae) is cut into 10 15cm strips, it is placed in autoclave, the water of 500L volume is added in reactor, add 45kg magnesium bicarbonate and 30kg magnesium magnesium carbonate, reactor parameter, reaction temperature 250 DEG C are set, reactor pressure 250MPa, reacts 55min；
(2) reaction terminates rear coarse filtration and obtains alginic acid magnesium crude extract；
(3) in alginic acid magnesium crude extract, add activated carbon adsorption decolouring, filter, it is thus achieved that the extracting solution just purified；
(4) extracting solution of preliminary purification by cationic exchange resin adsorption purify further, roguing, obtain the extracting solution of purification；
(5) adopting vacuum-concentrcted method, the extracting solution concentration to purification, parameter is vacuum 0.06MPa, temperature 90 DEG C, and concentration time is 22min.
(6) concentrated solution carries out spray drying, and the temperature of spray drying is 70 DEG C, and drying time is the 1.2h pressed powder obtaining alginic acid magnesium.
2, product viscosity index
Rotary viscosity under 20 DEG C of conditions of 1% glue of alginic acid magnesium prepared by said method is 7mPa.s.
Claims (7)
1. the production technology of a kind of ultra-low viscosity alginic acid magnesium of disclosure, its feature comprises the steps of
(1) water and the 15% compound magnesium salt of 5 times is cleaned, shredded, adds to Brown algae, is placed in degradation treatment in high temperature, autoclave, processes time 50-60min；
(2) coarse filtration obtains alginic acid magnesium crude extract；
(3) in alginic acid magnesium crude extract, add activated carbon adsorption decolouring, filter, it is thus achieved that the extracting solution just purified；
(4) extracting solution of preliminary purification is by ion exchange resin absorption purification further, roguing, obtains the extracting solution of purification；
(5) the extracting solution concentration of purification；
(6) concentrated solution carries out spray drying, obtains the pressed powder of alginic acid magnesium.
2. the production technology of a kind of ultra-low viscosity alginic acid magnesium according to claim 1, it is characterised in that: in described step (1), Brown algae mainly includes Thallus Laminariae (Thallus Eckloniae), Macrocystis pyrifera (L.) Ag., Alga Sgrgassi Enerves.
3. the production technology of a kind of ultra-low viscosity alginic acid magnesium according to claim 1, it is characterised in that: in described step (1) treatment temperature be 250 300 DEG C, processing pressure be 200 300MPa..
4. the production technology of a kind of ultra-low viscosity alginic acid magnesium according to claim 1, it is characterised in that: in described step (1), compound magnesium salt is one or more in magnesium bicarbonate, magnesium hydroxide, magnesium carbonate.
5. the production technology of a kind of ultra-low viscosity alginic acid magnesium according to claim 1, it is characterised in that: described step (4) ion exchange resin is cation exchange resin.
6. the production technology of a kind of ultra-low viscosity alginic acid magnesium according to claim 1, it is characterized in that: in described step (5), adopting vacuum-concentrcted, vacuum is 0.06 0.08MPa, concentration-temperature is 80-100 DEG C, and concentration time is 20 25min.
7. the production technology of a kind of ultra-low viscosity alginic acid magnesium according to claim 1, it is characterised in that: in described step (5), the temperature of spray drying is 60-75 DEG C, and drying time is 1 1.5h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201511024283.4A CN105754009A (en) | 2015-12-30 | 2015-12-30 | Production process of super-low-viscosity magnesium alginate |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201511024283.4A CN105754009A (en) | 2015-12-30 | 2015-12-30 | Production process of super-low-viscosity magnesium alginate |
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| CN105754009A true CN105754009A (en) | 2016-07-13 |
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| CN201511024283.4A Pending CN105754009A (en) | 2015-12-30 | 2015-12-30 | Production process of super-low-viscosity magnesium alginate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115651094A (en) * | 2022-11-18 | 2023-01-31 | 青岛海之林生物科技开发有限公司 | Low-calcium and low-viscosity sodium alginate and preparation method thereof |
| CN115850532A (en) * | 2022-12-14 | 2023-03-28 | 青岛海之林生物科技开发有限公司 | Water-soluble neutral stable magnesium alginate prepared by supercritical carbon dioxide and preparation method thereof |
-
2015
- 2015-12-30 CN CN201511024283.4A patent/CN105754009A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115651094A (en) * | 2022-11-18 | 2023-01-31 | 青岛海之林生物科技开发有限公司 | Low-calcium and low-viscosity sodium alginate and preparation method thereof |
| CN115850532A (en) * | 2022-12-14 | 2023-03-28 | 青岛海之林生物科技开发有限公司 | Water-soluble neutral stable magnesium alginate prepared by supercritical carbon dioxide and preparation method thereof |
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