CN103923223A - Method for extracting fucoidan from fresh kelp blanching wastewater - Google Patents
Method for extracting fucoidan from fresh kelp blanching wastewater Download PDFInfo
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Abstract
The present invention provides a method for extracting fucoidan by using fresh kelp blanching wastewater containing a certain nutrient. According to the present invention, separation of the fucoidan and other impurities is achieved through pH value adjustment, and characteristics of low equipment investment, low maintenance cost and long service life are provided; the obtained material can be stored for a long time after alkali coagulation precipitation drying so as to overcome the disadvantage of strong seasonal production property of fresh kelp blanching wastewater; and the obtained fucoidan has characteristics of low impurity content and high quality.
Description
Technical field
The invention belongs to Living marine resources and utilize field, be specifically related to a kind of method of extracting algal polysaccharide sulfate from fresh sea-tangle blanching waste water.
Background technology
Laminaria culture output and the process scale of China all occupy first place in the world.According to statistics, China in 2010 sea-tangle annual production reaches 88.4 ten thousand tons (with dry weight basis), accounts for 57.3% of China's marine alga ultimate production.Within 2010, China's algae processed goods output reaches 94.6 ten thousand tons, and wherein, the annual production of salt marsh sea-tangle is about 420,000 tons, and annual value of production exceedes 1,200,000,000 yuan, mainly concentrates on the ground such as Shandong, Fujian, Liaoning.The processing of salt marsh sea-tangle is the important component part of China's kelp food processing.By just from the fresh sea-tangle of mariculture district results with 80～90 DEG C of of short duration blanchings of hot water, through cooling, draining, mix dehydration of salt and obtain the crude product of salt marsh sea-tangle, then can become launch products or outlet through the arrangement such as chopping or knotting.
In fresh sea-tangle blanching processing waste water, available affluent resources are out in the cold for a long time.Spread all over the blanching sea-tangle processing line in laminaria culture region producing a large amount of waste water of up to a million tons that produce season, be directly discharged into marine without any processing.In these waste water, contain iodine, algal polysaccharide sulfate, N.F,USP MANNITOL, laminine, fucoxanthin etc., wherein iodine average content is 400mg/kg, and algal polysaccharide sulfate (claiming again fucoidin, fucoidan) average content is 280mg/kg.In addition, in waste water, also contain the principal pollutant such as suspended substance (SS), nitrate nitrogen, nitrite nitrogen, total ammonia nitrogen.If these waste water are not recycled and are processed and directly discharge, bring on the one hand environmental pollution, wherein inorganic the and organic composition of contained iodine and various high reactivity, high added value runs off in a large number on the other hand, has caused the great wasting of resources.
Algal polysaccharide sulfate (fucoidan) is a class sulfated polysaccharides, is present in brown alga, first from palmate sea-tangle, is extracted in 1913 by Kylin.Kylin will isolate L-fucose after extract hydrolysis, he is by this polysaccharide called after fucoidin, now generally name as fucoidan according to the nomenclature mo of polysaccharide, Chinese is fucoidin, fucoidin, fucosan, fucoidan, fucoidin or algal polysaccharide sulfate.Now people have comparatively clearly and understand the composition of algal polysaccharide sulfate, and it is the very complicated polysaccharide of a class chemical composition and structure, taking Fucose and sulfate as main, along with the kind difference of algae also contains other compositions such as semi-lactosi, wood sugar, uronic acid.Sea-tangle Fucoidan is made up of monose such as Fucose, semi-lactosi, wood sugar, glucuronic acid, pectinoses.Taking Fucose and semi-lactosi as main, Fucose and semi-lactosi are probably at 3:1.
About the structure of fucoidan, most research datas shows that fucoidan is mainly the L-fucose composition connecting with α-(1 → 3), sulfation occurs in C4 or C2 position, and the L-fucose that part Study shows existence part (1 → 2) connection is as side chain.There is similarity with the algae algal polysaccharide sulfate structure of restricting in upper figure.But there is part ethanoyl in rope algae.And different substituents to roll into a ball shared ratio also different.Certainly in molecule, also have the monose such as semi-lactosi, wood sugar, rhamnosyl, semi-lactosi may participate in the composition of main chain, and wood sugar, rhamnosyl etc. are to exist with the form of side chain.
Existing many sections of documents disclose preparation method and the pharmaceutical applications thereof of algal polysaccharide sulfate.The clear 46-2248 of Japanese Patent adopts n-Hexadecane pyridinium chloride or hexadecane trimethyl ammonium bromide and algal polysaccharide sulfate to be reacted into quaternary amine mixture, recycle the dissolubility difference of this mixture to salt, by ethanol, methyl alcohol and ion exchange resin treatment, purifying is removed algin, neutral polysaccharide and other impurity, and obtains the algal polysaccharide sulfuric acid acid esters of comparison purifying.CN1129109A discloses by dry kelp soaking, for several times filtrations, secondary extraction using alcohol, washing with alcohol, has coordinated the alkali condensation method of adjusting PH scope etc.CN1344565A discloses another kind of preparation method, comprises the steps such as raw materials pretreatment, temperature control stirring lixiviate, centrifugal, concentrated, ethanol precipitation, dehydrated alcohol dehydration.CN1560086A discloses a kind of preparation method of fucosan sulfate of high sulfuric content, with hot water or sour water lixiviate brown alga, make the extracting solution containing fucoidan sulfuric ester, the weight percentage that this extracting solution is concentrated into polysaccharide is 2-10%, adjusts PH5-8, adds chitosan solution to stir, centrifugal or cross collecting precipitation, to precipitate for 5-10 times of salts solution and extract 2-4 time, clear liquid is collected in centrifugal or filtration, by this clear liquid dialysis or ultrafiltration desalination.In addition, CN1670028A, CN1392160A, CN1197674A also disclose respectively and have adopted the method such as flocculation to prepare Sargassum polysaccharides.
Algal polysaccharide sulfate has anticoagulation, improves immunizing power, antitumor, hypoglycemic, radioprotective, inhibition ascitic tumor isoreactivity, and CN1547478A discloses its purposes in treatment adhesion, sacroiliitis and psoriasis.We have become algal polysaccharide sulfate exploitation the medicine for the treatment of renal failure, and algal polysaccharide sulfate also has huge development prospect as healthcare products and cosmetic material.
All directly adopt marine alga as extracting raw material because original algal polysaccharide sulfate extracts, if not in conjunction with marine alga comprehensive utilization, extract separately and make the preparation cost of algal polysaccharide sulfate high.In fresh sea-tangle blanching water, contain certain algal polysaccharide sulfate and other nutritive substance, develop fresh sea-tangle blanching water conservancy use technology necessary.
Summary of the invention
For addressing the above problem, the invention provides a kind of method of extracting algal polysaccharide sulfate from fresh sea-tangle blanching waste water, to make full use of the nutritive ingredient containing in fresh sea-tangle blanching waste water.
For achieving the above object, technical scheme of the present invention is:
A method of extracting algal polysaccharide sulfate from fresh sea-tangle blanching waste water, comprises the following steps:
(1), in fresh sea-tangle blanching waste water, add solid base or alkaline solution, it is 9-10 that the pH value of blanching water is adjusted to pH, makes to occur precipitation;
(2), by filtering separation supernatant liquor and precipitation, collecting precipitation;
(3), will precipitate dryly, dried precipitation can be preserved for a long time;
(4), precipitation acid adding, stir make it dissolve, regulate pH to being less than or equal to 2, at this moment precipitation be partly dissolved, form suspension liquid;
(5) suspension liquid is filtered, collect filtrate;
(6) filtrate water is diluted to pH>2, and separating desalination is collected the film trapped fluid after desalination;
(7) trapped fluid being further concentrated into proportion is 1.03-1.08;
(8) concentrated solution spraying is dry, obtains algal polysaccharide sulfate powder;
Or concentrated solution adopts ethanol precipitation processing; More than 65%, generate precipitation by adding ethanol in concentrated solution to ethanol final concentration; Precipitation leaves standstill more than 12 hours, and precipitation drying under reduced pressure obtains algal polysaccharide sulfate.
Preferably, in described step (1), regulate fresh sea-tangle blanching waste water to alkalescence with alkali, alkali used comprises sodium hydroxide, potassium hydroxide, sodium carbonate or salt of wormwood.
Preferably, described step (4) precipitation acid adding, regulates pH<2, and acid used is hydrochloric acid, sulfuric acid or nitric acid, and institute's acid adding concentration range is 0.01-0.5 mol/L.
Membrane sepn step described in preferred described step (7), adopts ultrafiltration, nanofiltration or electrodialysis.
Preferably, the enrichment step described in described step (8), adopts concentrating under reduced pressure or evaporation concentration.
Tool of the present invention has the following advantages:
1, the present invention has set up one and has utilized fresh sea-tangle blanching waste water extraction algal polysaccharide sulfate, not only can solve processing and the emission problem of fresh sea-tangle blanching waste water, and turn waste into wealth, and has set up a kind of method of low cost extraction algal polysaccharide sulfate.Blanching waste water supernatant liquor after alkaline purification simultaneously can be further used for extracting iodine.Can realize the comprehensive utilization of fresh sea-tangle blanching waste water, the waste water after utilization is realized qualified discharge, has avoided its pollution to environment;
2, present method mainly realizes algal polysaccharide sulfate by the adjusting of pH and separates with other impurity, is not subject to that impurity disturbs, facility investment is low, maintenance cost is low, long service life.Alkali retrogradation can be preserved after forming sediment and being dried for a long time, overcomes fresh sea-tangle blanching waste water and produces seasonal strong shortcoming.The algal polysaccharide sulfate foreign matter content obtaining is few, and quality is high.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment are only not used in and limit the scope of the invention for the present invention is described.In addition should be understood that, after having read content of the present invention, those skilled in the art can make various changes or modifications the present invention, these equivalent form of values fall within equally the application the scope that limits of attached claims.
Embodiment 1,
Get 10 L sea-tangle blanching waste waters, under agitation slowly add the sodium hydroxide solution of 10 mol/L, regulate pH value to 10, slowly occur condensation product (precipitation).Leave standstill 5 hours, silk cover filtering, collecting precipitation.Precipitation is dried, obtain dry substance 7.5g.Dry substance is placed in to beaker, adds the hydrochloric acid of 250ml 0.01 mol/L, stir solvent 4 hours, taking diatomite as flocculating aids suction filtration, collect supernatant liquor 230 mL.10 times of distilled water dilutings for supernatant liquor, surveying pH value is 3.2, and ultra-filtration membrane trapped fluid 200 mL are collected in ultrafiltration desalination, and 60 DEG C are evaporated to 35 mL, and concentrated solution proportion is 1.03.Concentrated solution add in edible ethanol to concentration be 70%, production brown precipitation.Precipitation hold over night, with 95% washing with alcohol precipitation, by throw out vacuum-drying, obtains algal polysaccharide sulfate 2.5g.It is 31.2% that chemical composition is analyzed Fucose content in algal polysaccharide sulfate, sulfate content 30.4%.
Embodiment 2,
Get 10 L sea-tangle blanching waste waters, under agitation slowly add the sodium carbonate solution of 5 mol/L, regulate pH value to 9, slowly occur condensation product (precipitation).Precipitation leaves standstill 2 hours, silk cover filtering, collecting precipitation.Precipitation is dried, obtain dry substance 8.2g.Dry substance is placed in to beaker, adds the hydrochloric acid of 810ml 0.02 mol/L, stir solvent 8 hours, taking diatomite as flocculating aids suction filtration, collect supernatant liquor 810 mL.5 times of distilled water dilutings for supernatant liquor, surveying pH value is 3.0, and ultra-filtration membrane trapped fluid 200 mL are collected in ultrafiltration desalination, and 60 DEG C are evaporated to 25 mL, and concentrated solution proportion is 1.05.Concentrated solution add in edible ethanol to concentration be 70%, production brown precipitation.Precipitation hold over night, with 95% washing with alcohol precipitation, by throw out vacuum-drying, obtains algal polysaccharide sulfate 2.2g.It is 32.5% that chemical composition is analyzed Fucose content in algal polysaccharide sulfate, sulfate content 31.0%.
Embodiment 3,
Get 50 L sea-tangle blanching waste waters, under agitation slowly add solid state hydrogen potassium oxide, regulate pH value to 9.8, slowly occur condensation product (precipitation).Leave standstill 12 hours, silk cover filtering, collecting precipitation.Precipitation is dried, obtain dry substance 42.3g.Hydrochloric acid by dry substance with 2000 ml 0.05 mol/L, stirs solvent 4 hours, taking diatomite as flocculating aids suction filtration, collects supernatant liquor 1950 mL.10 times of distilled water dilutings for supernatant liquor, surveying pH value is 2.4, and ultra-filtration membrane trapped fluid 400 mL are collected in ultrafiltration desalination, and 60 DEG C are evaporated to 110 mL, and concentrated solution proportion is 1.04.Concentrated solution spraying is dry, obtains algal polysaccharide sulfate powder 10.3 g.It is 28.5% that chemical composition is analyzed Fucose content in algal polysaccharide sulfate, sulfate content 29.4%.
Embodiment 4,
Get 50 L sea-tangle blanching waste waters, under agitation slowly add the sodium hydroxide solution of 3 mol/L, regulate pH value to 9.1, slowly occur condensation product (precipitation).Leave standstill 12 hours, silk cover filtering, collecting precipitation.Precipitation is dried, obtain dry substance 38.4g.Hydrochloric acid by dry substance with 2000 ml 0.1 mol/L, stirs solvent 12 hours, taking diatomite as flocculating aids suction filtration, collects supernatant liquor 1950 mL.20 times of distilled water dilutings for supernatant liquor, surveying pH value is 2.1, nanofiltration membrane trapped fluid 400 mL are collected in nanofiltration desalination, evaporation concentration to 66 mL, concentrated solution proportion is 1.08.Concentrated solution spraying is dry, obtains algal polysaccharide sulfate powder 9.7 g.It is 29.3% that chemical composition is analyzed Fucose content in algal polysaccharide sulfate, sulfate content 31.5%.
In the above-described embodiments,
The pH value range regulation of blanching waste water is any number between 9-10, makes to occur precipitation;
In precipitation acid adding step, stir and make it to dissolve, and regulate pH to any number that is less than or equal to 2, at this moment precipitation is partly dissolved, and forms suspension liquid;
By in the step of filtrate water dilution, make pH>2, separating desalination, collects the film trapped fluid after desalination;
By trapped fluid further in concentrated step, by any number between its proportion simmer down to 1.03-1.08;
In the time that concentrated solution adopts ethanol precipitation to process; More than 65%, generate precipitation by adding ethanol in concentrated solution to ethanol final concentration; Precipitation leaves standstill more than 12 hours, and precipitation drying under reduced pressure obtains algal polysaccharide sulfate.
Regulate fresh sea-tangle blanching waste water to alkalescence with alkali in step (1) time, alkaline solution used is sodium hydroxide or sodium carbonate solution, and wherein naoh concentration scope is 3-20 mol/L; Sodium carbonate solution concentration range is 2-10 mol/L.
In the link of step (4) precipitation acid adding, regulate pH<2, acid used is hydrochloric acid or nitric acid, institute's acid adding concentration range is 0.01-0.5 mol/L.
At the enrichment step described in step (8), adopt concentrating under reduced pressure or evaporation concentration or adopt concentrating under reduced pressure.
Tool of the present invention has the following advantages:
1, the present invention has set up one and has utilized fresh sea-tangle blanching waste water extraction algal polysaccharide sulfate, not only can solve processing and the emission problem of fresh sea-tangle blanching waste water, and turn waste into wealth, and has set up a kind of method of low cost extraction algal polysaccharide sulfate.Blanching waste water supernatant liquor after alkaline purification simultaneously can be further used for extracting iodine.Can realize the comprehensive utilization of fresh sea-tangle blanching waste water, the waste water after utilization is realized qualified discharge, has avoided its pollution to environment;
2, present method mainly realizes algal polysaccharide sulfate by the adjusting of pH and separates with other impurity, is not subject to that impurity disturbs, facility investment is low, maintenance cost is low, long service life.Alkali retrogradation can be preserved after forming sediment and being dried for a long time, overcomes fresh sea-tangle blanching waste water and produces seasonal strong shortcoming.The algal polysaccharide sulfate foreign matter content obtaining is few, and quality is high.
Be more than the description to the embodiment of the present invention, by the above-mentioned explanation to the disclosed embodiments, make professional and technical personnel in the field can realize or use the present invention.To be apparent for those skilled in the art to the multiple amendment of these embodiment, General Principle as defined herein can, in the situation that not departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention will can not be restricted to these embodiment shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (5)
1. a square h method of extracting algal polysaccharide sulfate from fresh sea-tangle blanching waste water, is characterized in that, comprises the following steps:
(1), in fresh sea-tangle blanching waste water, add solid base or alkaline solution, it is 9-10 that the pH value of blanching waste water is adjusted to pH, makes to occur precipitation;
(2), by filtering separation supernatant liquor and precipitation, collecting precipitation;
(3), will precipitate dryly, dried precipitation can be preserved for a long time;
(4), precipitation acid adding, stir make it dissolve, regulate pH to being less than or equal to 2, at this moment precipitation be partly dissolved, form suspension liquid;
(5) suspension liquid is filtered, collect filtrate;
(6) filtrate water is diluted to pH>2, and separating desalination is collected the film trapped fluid after desalination;
(7) trapped fluid being further concentrated into proportion is 1.03-1.08;
(8) concentrated solution spraying is dry, obtains algal polysaccharide sulfate powder;
Or concentrated solution adopts ethanol precipitation processing; More than 65%, generate precipitation by adding ethanol in concentrated solution to ethanol final concentration; Precipitation leaves standstill more than 12 hours, and precipitation drying under reduced pressure obtains algal polysaccharide sulfate.
2. the method for extracting algal polysaccharide sulfate from fresh sea-tangle blanching waste water according to claim 1, it is characterized in that, in described step (1), regulate fresh sea-tangle blanching waste water to alkalescence with alkali, alkali used comprises sodium hydroxide, potassium hydroxide, sodium carbonate or salt of wormwood.
3. the method for extracting algal polysaccharide sulfate from fresh sea-tangle blanching waste water according to claim 1, it is characterized in that, described step (4) precipitation acid adding, regulates pH<2, acid used is hydrochloric acid, sulfuric acid or nitric acid, and institute's acid adding concentration range is 0.01-0.5 mol/L.
4. the method for extracting algal polysaccharide sulfate from fresh sea-tangle blanching waste water according to claim 1, is characterized in that, the separating desalination step described in described step (7), and described membrane sepn can adopt ultrafiltration, nanofiltration or electrodialysis.
5. the method for extracting algal polysaccharide sulfate from fresh sea-tangle blanching waste water according to claim 1, is characterized in that, the enrichment step described in described step (8) adopts concentrating under reduced pressure or evaporation concentration.
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Cited By (8)
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| CN104744607A (en) * | 2015-04-22 | 2015-07-01 | 青岛正大海尔制药有限公司 | Method for preparing polysaccharide sulfate through nanofiltration technology |
| CN104774278A (en) * | 2015-04-22 | 2015-07-15 | 青岛正大海尔制药有限公司 | Method for preparing polysaccharide sulfate by virtue of electrochemical reaction |
| CN104829386A (en) * | 2015-06-04 | 2015-08-12 | 威海恒源生物工程开发有限公司 | Seaweed water-soluble fertilizer and preparation method thereof |
| CN106916234A (en) * | 2017-02-22 | 2017-07-04 | 四川绿沃创新环保工程有限公司 | A kind of extraction and separation process of algal polysaccharide sulfate |
| CN107266606A (en) * | 2017-08-23 | 2017-10-20 | 山东大学 | The new technology of fucoidan is extracted in a kind of waste liquid from kelp processing |
| CN107382667A (en) * | 2017-07-26 | 2017-11-24 | 中国水产科学研究院黄海水产研究所 | The cycles, economized processing method of dissolved organic matter in one main laminaria blanching water |
| CN107382666A (en) * | 2017-07-26 | 2017-11-24 | 中国水产科学研究院黄海水产研究所 | The efficient energy-saving extracting method of dissolved organic matter in one main laminaria blanching water |
| CN107881207A (en) * | 2017-11-19 | 2018-04-06 | 荣成海锐芯生物科技有限公司 | A kind of preparation method of the laminarin of low content of iodine |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104744607A (en) * | 2015-04-22 | 2015-07-01 | 青岛正大海尔制药有限公司 | Method for preparing polysaccharide sulfate through nanofiltration technology |
| CN104774278A (en) * | 2015-04-22 | 2015-07-15 | 青岛正大海尔制药有限公司 | Method for preparing polysaccharide sulfate by virtue of electrochemical reaction |
| CN104829386A (en) * | 2015-06-04 | 2015-08-12 | 威海恒源生物工程开发有限公司 | Seaweed water-soluble fertilizer and preparation method thereof |
| CN104829386B (en) * | 2015-06-04 | 2018-01-26 | 威海恒源生物工程开发有限公司 | A kind of marine alga water-soluble fertilizer and preparation method thereof |
| CN106916234A (en) * | 2017-02-22 | 2017-07-04 | 四川绿沃创新环保工程有限公司 | A kind of extraction and separation process of algal polysaccharide sulfate |
| CN107382667A (en) * | 2017-07-26 | 2017-11-24 | 中国水产科学研究院黄海水产研究所 | The cycles, economized processing method of dissolved organic matter in one main laminaria blanching water |
| CN107382666A (en) * | 2017-07-26 | 2017-11-24 | 中国水产科学研究院黄海水产研究所 | The efficient energy-saving extracting method of dissolved organic matter in one main laminaria blanching water |
| CN115557828A (en) * | 2017-07-26 | 2023-01-03 | 中国水产科学研究院黄海水产研究所 | Method for treating soluble organic matters in kelp blanching water |
| CN107266606A (en) * | 2017-08-23 | 2017-10-20 | 山东大学 | The new technology of fucoidan is extracted in a kind of waste liquid from kelp processing |
| CN107266606B (en) * | 2017-08-23 | 2020-03-27 | 山东大学 | New process for extracting fucosan sulfate from kelp processing waste liquid |
| CN107881207A (en) * | 2017-11-19 | 2018-04-06 | 荣成海锐芯生物科技有限公司 | A kind of preparation method of the laminarin of low content of iodine |
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Application publication date: 20140716 |