CN100425622C - Method for extracting fucoidin by comprehensively utilizing kelp - Google Patents
Method for extracting fucoidin by comprehensively utilizing kelp Download PDFInfo
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- CN100425622C CN100425622C CNB2006100689683A CN200610068968A CN100425622C CN 100425622 C CN100425622 C CN 100425622C CN B2006100689683 A CNB2006100689683 A CN B2006100689683A CN 200610068968 A CN200610068968 A CN 200610068968A CN 100425622 C CN100425622 C CN 100425622C
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- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 claims abstract description 21
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 39
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 31
- 239000007788 liquid Substances 0.000 claims description 27
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- 235000021110 pickles Nutrition 0.000 claims description 17
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 238000000926 separation method Methods 0.000 claims description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
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- 241001466453 Laminaria Species 0.000 claims description 4
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 4
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 4
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- 235000003891 ferrous sulphate Nutrition 0.000 claims description 3
- 239000011790 ferrous sulphate Substances 0.000 claims description 3
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 3
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 3
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 3
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- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 2
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- PNNNRSAQSRJVSB-SLPGGIOYSA-N Fucose Natural products C[C@H](O)[C@@H](O)[C@H](O)[C@H](O)C=O PNNNRSAQSRJVSB-SLPGGIOYSA-N 0.000 claims 1
- SHZGCJCMOBCMKK-DHVFOXMCSA-N L-fucopyranose Chemical compound C[C@@H]1OC(O)[C@@H](O)[C@H](O)[C@@H]1O SHZGCJCMOBCMKK-DHVFOXMCSA-N 0.000 claims 1
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Landscapes
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention provides a process for extracting fucoidin by comprehensively utilizing kelp, which can solve the problems of low leaching rate of iodine, mannitol and fucoidin, high preparation cost, poor comprehensive utilization effect and the like in the prior art. The kelp is comprehensively utilized, secondary soaking is adopted, the leaching rates of iodine, mannitol and fucoidin are improved, the impurity content of kelp is reduced, and the vegetable washing cost in the process of extracting algin is reduced. For the water quality deterioration caused by enhancing stirring, the flocculation treatment mode is adopted to purify the water quality, on one hand, the water quality purification after alkali refining is further improved, the extraction conditions of iodine and mannitol are improved, and the product yield is improved; on the other hand, the removal of the flocculation impurities greatly improves the purity of the alkali refining scum containing the rock algae polysaccharide, and simplifies the subsequent purification process. The method of the invention integrally improves the extraction conditions of all products, reduces the production cost, obviously improves the extraction rate of iodine, mannitol and fucoidin, and greatly improves the comprehensive utilization value of limited seaweed resources.
Description
Technical field
The present invention relates in the process of sea-tangle processing algin, iodine, N.F,USP MANNITOL, the method for fucoidin is produced in the coproduction of comprehensive utilization waste, has both utilized the kelp soaking scale to refine the method that isolating scum silica frost is produced fucoidin.
Background technology
Fucoidin is algal polysaccharide again, is institute's inherent iuntercellular polysaccharide in the brown alga, is present in the cell walls matrix.Its function may be when the time of low water frond is exposed to the anti-effect of doing of the moisture absorption to be arranged in the atmosphere.Studies show that algal polysaccharide has the pharmaceutical activity of certain lipidemia and inhibition tumour, caused pharmacy research staff's concern in recent years, that product can be produced is antitumor, antiviral, the natural radioactivity medicine of reducing blood-fat, be used for the treatment of tumour, cardiovascular disease and renal function disease, also can produce the healthcare products of anti-oxidant, reducing blood-fat, raising body immunity.
Present fucoidin preparation has directly extracts from brown alga and two kinds of methods of brown alga comprehensive utilization extraction.The former does not obviously possess cost advantage, deficiency in economic performance, thereby fail to form suitability for industrialized production.
The latter has utilized existing alkali refining waste residue to extract in the brown alga course of processing fully, but exists following deficiency:
1. original pickles method is in order to guarantee the water quality clarity after the pickles scale refines, should not too stir during pickles, to prevent that fucoidin and other impurity strippings from entering in the water, had a strong impact on the leaching yield of iodine, N.F,USP MANNITOL, fucoidin so on the one hand, increased the content of impurity in the dish on the other hand, increased algin and extracted the washing cost of using the sea-tangle dish.
2. a large amount of impurity that original alkali refining purification process will soak in the water enter in the scum silica frost in the lump with the flocculation of fucoidin, and the follow-up purification of fucoidin is brought very big difficulty, have increased cost for purification greatly.
Above-mentioned deficiency has influenced the popularization of directly extracting the fucoidin method from brown alga, can't form large-scale production, and the brown alga comprehensive utilization is extracted fucoidin and also have significant limitation in limited actual production.
How solving the problem of above-mentioned existence, then is the design problem that the present invention faced.
Summary of the invention
The invention provides main laminaria comprehensive utilization and extract the method for fucoidin, the leaching yield that it can solve iodine that prior art exists, N.F,USP MANNITOL, fucoidin is low, produces the cost height, and problem such as comprehensive utilization weak effect.
In order to reach the purpose that solves the problems of the technologies described above, technical scheme of the present invention is, the technology of fucoidin is extracted in the comprehensive utilization of one main laminaria, it is characterized in that utilizing the waste that produces in the process of sea-tangle for raw material production algin, iodine, N.F,USP MANNITOL to produce fucoidin, this preparation method comprises the following order step:
(1). the pickles operation, take the mode of twice cover bubble to soak the sea-tangle that cuts through overdrying with 8-10 times of tap water, so that leach more iodine, N.F,USP MANNITOL, fucoidin in the water.The first pass of every batch of sea-tangle soaks water, enters cleaning section; Soak water for two times and be used to do the of next batch dish-carry out pickles all over water; Sea-tangle is used to extract algin;
(2). cleaning section, the inorganic water conditioner of adding forms insolubles after soaking depositing in water to fall separation, adds flocculation agent with the intensive throw out of insolubles flocculation formation, carries out rough purification, removal of impurities, emits clear liquid to the alkali refining jar, and residue is drained;
(3). purify waste water in alkali refining jar alkali refining flocculation separation fucoidin scum silica frost, emit clear liquid and be used to extract iodine and N.F,USP MANNITOL, scum silica frost is retracted to retort with vacuum;
(4). the carbohydrate gum scum silica frost is adjusted the dissolving of pH value, and heat to boil and carry;
(5). the leach cooking liquid natural subsidence to layering, is discarded precipitation, supernatant liquor is filtered to see-through 〉=30cm with flocculating aids;
(6). filtered liquid vacuum concentration, cooling, crystallization, separation desalination and N.F,USP MANNITOL;
(7). it is 25%-30% that above-mentioned clear liquid adds ethanol to alcohol concn, and natural subsidence discards precipitated impurities to layering behind the mixing;
(8). clear liquid is transferred pH value 1-3, acid degradation;
(9). with adding ethanol to alcohol concn in the degradation solution is 65-80%, and mixing, alcohol are analysed;
(10). natural subsidence and centrifugal the combining of machinery, alcohol analysed thing separates and washing with alcohol;
(11). the dry alcohol of sudden strain of a muscle formula is analysed thing, pulverizes and promptly gets the fucoidin product.
In the present invention, also have following technical characterictic: described in the pickles operation, behind the input sea-tangle, stirring replaces at least once with Jing Pao when soaking at every turn, stirs 0.5-3 minute; Quiet bubble 15-45 minute.
In the present invention, also have following technical characterictic: inorganic water conditioner adopts at least a in bodied ferric sulfate, ferrous sulfate, Tai-Ace S 150, polymerize aluminum chloride, the poly-ferric chloride, working concentration is 100-150ppm, flocculation agent is conventional polyacrylamide macromolecular compound, and working concentration is 5-10ppm.
In the present invention, also have following technical characterictic: the described alkali refining of purifying waste water uses caustic soda or white lime.
In the present invention, also have following technical characterictic: dissolving is extracted to the carbohydrate gum scum silica frost, adopts hydrochloric acid to regulate scum silica frost pH value 4-5, heats 75-90 ℃, boils and carries.
In the present invention, also have following technical characterictic: described flocculating aids is diatomite or perlite.
In the present invention, also have following technical characterictic: 3～5 times of described filtered liquid vacuum concentration make the concentrated solution solid content reach 40～50%.
Described step (1) pickles technology need change according to the sea-tangle raw materials quality and suitably adjust, and pickles adopt and stir and quiet bubble bonded mode, and based on Jing Pao, the mode of secondary cover bubble guarantees that leaching yield brings up to more than 90% from original 70%.
Described step (2) purification process fibrous root carries out the technology adjustment according to change of water quality, comprises that the complete measure of physics sedimentation, flocculation, separation etc. one cover realizes that it purifies purpose, and the foreign matter content of purifying waste water drops to original below 20%.
Described step (3) alkali refining of purifying waste water can use caustic soda or white lime to reach the purpose of abundant flocculation.
Described step (4) vacuum drawn alkali refining scum silica frost in conjunction with the characteristics of the mobile difference of scum silica frost, is realized the isolating automatization of scum silica frost, the dilution of having avoided the slagging bath to cause, and vacuum exhaust simultaneously obviously reduces the scum silica frost air content, and volume reduces half, is convenient to subsequent disposal.
Described step (6) filtering equipment is Specialty Design, has realized the automatization and the serialization of producing, and selects for use several diatomaceous models to carry out rational assembly, has guaranteed filter quality and efficient.
Described step (11) is used natural subsidence and the centrifugal separation method that combines of machinery, it is first natural subsidence separation of supernatant, centrifugation sediment again, centrifugal waste liquid is further settlement separate, separate with method after the throw out washing with alcohol, simplified equipment and dropped into expense, guaranteed that again extraction rate reached is more than 95%.
Described step (12) sudden strain of a muscle formula drying is the TRANSIENT HIGH TEMPERATURE drying, has both guaranteed quality product, and efficient is high again, is fit to suitability for industrialized production.Fucoidin is to thermo-responsive, easy deliquescence, and the long-time high temperature of common desiccating method easily causes the sex change of product; The general low-temperature vacuum drying method that adopts, drying efficiency is low, the cost height.
As sea-tangle comprehensive utilization, adopt secondary cover bubble, improve iodine, N.F,USP MANNITOL, fucoidin leaching yield, reduce the sea-tangle foreign matter content, reduced and washed the dish cost in the algin leaching process.
For the water quality deterioration of strengthening stirring and causing, adopt the mode of flocculation treatment to purify water, the result further improves alkali refining after water quality on the one hand, improves the extraction conditions of iodine and N.F,USP MANNITOL, improves product yield; On the other hand, the removal of flocculated impurities makes the alkali refining scum silica frost purity that contains fucoidin greatly improve, and simplifies follow-up purifying technique.
Compared with the prior art, the inventive method, integral body improved all products extraction conditions, reduced production cost, simultaneously the extraction yield of iodine, N.F,USP MANNITOL, fucoidin all is significantly improved, and has improved the comprehensive utilization value of limited marine algae resource to a greater extent.
Embodiment
Embodiment 1
1.. dried sea-tangle 500kg, cut to about 20cm length through beet slicer, add last time two times water of cover bubble in the water washing tank, add 7000kg with tap water, drop into sea-tangle, stirred 1 minute, quiet bubble 30 minutes is with method stirring, Jing Pao, pickles are 90 minutes altogether, the about 2000kg of sea-tangle suction, the 5000kg that discharges water is used for purifying treatment; Sea-tangle behind the control water adds tap water 5000kg, adds solubility promoter 10kg, stirs 1 minute, and quiet bubble is after 15 minutes, and with method stirring, Jing Pao, pickles are 30 minutes altogether, discharge water, and is used for the dried sea-tangle of cover bubble next time; Sea-tangle is used to extract algin.
2. overlap soaked 5000kg, precipitation, supernatant liquor is squeezed into purification pot, slowly add the polyaluminium sulfate 7.5kg of concentration 10% with water, left standstill 30 minutes, added 0.1% anionic polyacrylamide flocculation agent 25kg flocculation 10-15 minute, emit clear liquid to the alkali refining jar, residue is drained.
3. alkali refining jar clear liquid turn on pump circulation foaming slowly adds caustic soda to Ph value 11.5 with pump intake, leaves standstill floating 1h, emits clear liquid and is used to extract iodine and N.F,USP MANNITOL, and scum silica frost is retracted to retort with vacuum.
4. open retort and stir, regulate scum silica frost pH value 4-5 with hydrochloric acid, stirring heating is boiled for 85 ℃ and is carried 1h.
5. behind the natural subsidence 6h, separation of supernatant, diatomite filtration.
6. filtered liquid is concentrated in vacuo to solid concentration 40%, crystallisation by cooling, centrifugation desalination and N.F,USP MANNITOL.
7. to add ethanol to alcohol concn be 25%-30% to clear liquid, leaves standstill the 2h precipitation behind the mixing, separates removal of impurities.
8. clear liquid is transferred pH value 3 with hydrochloric acid, heats 80 ℃ and keeps the 4h degraded.
9. adding ethanol to alcohol concn is 80%, and mixing staticly settles 2h, separation of supernatant, and alcohol is analysed the thing centrifugation and washed with method with 80% ethanol, and is centrifugal.
10. dodge the dry alcohol of formula and analyse thing, pulverize and promptly get the fucoidin crude product.
Embodiment 2
1. dried sea-tangle 500kg, cut to about 20cm length through beet slicer, add last time two times water of cover bubble in the water washing tank, add 6000kg with tap water, drop into sea-tangle, stirred 1 minute, quiet bubble 30 minutes is with method stirring, Jing Pao, pickles are 90 minutes altogether, the about 2000kg of sea-tangle suction, the 4000kg that discharges water is used for purifying treatment; Sea-tangle behind the control water adds tap water 5000kg, stirs 1 minute, and quiet bubble is after 15 minutes, and with method stirring, Jing Pao, pickles are 45 minutes altogether, discharge water, and is used for the dried sea-tangle of cover bubble next time; Sea-tangle is used to extract algin.
2. overlap soaked 4000kg, precipitation, supernatant liquor is squeezed into purification pot, slowly adds the bodied ferric sulfate 7kg of concentration 10% with water, leaves standstill 30 minutes, adds 0.1% anionic polyacrylamide flocculation agent 40kg flocculation 15 minutes, emits clear liquid to the alkali refining jar, and residue is drained.
3. alkali refining jar clear liquid turn on pump circulation foaming slowly adds emulsive white lime to Ph value 10 with pump intake, leaves standstill floating 1h, emits clear liquid and is used to extract iodine and N.F,USP MANNITOL, and scum silica frost is retracted to retort with vacuum.
Other step is with embodiment 1
Embodiment 3
4. dried sea-tangle 500kg, cut to about 20cm length through beet slicer, add last time two times water of cover bubble in the water washing tank, add 7000kg with tap water, drop into sea-tangle, stirred 1 minute, quiet bubble 30 minutes is with method stirring, Jing Pao, pickles are 90 minutes altogether, the about 2000kg of sea-tangle suction, the 5000kg that discharges water is used for purifying treatment; Sea-tangle behind the control water adds tap water 5000kg, adds solubility promoter 10kg, stirs 1 minute, and quiet bubble is after 15 minutes, and with method stirring, Jing Pao, pickles are 45 minutes altogether, discharge water, and is used for the dried sea-tangle of cover bubble next time; Sea-tangle is used to extract algin.
5. overlap soaked 5000kg, precipitation, supernatant liquor is squeezed into purification pot, slowly add the ferrous sulfate 10kg of concentration 10% with water, left standstill 30 minutes, added 0.1% anionic polyacrylamide flocculation agent 25kg flocculation 15 minutes, impurity floats to the surface, left standstill floating 20 minutes, and emitted clear liquid to the alkali refining jar, residue is drained.
Other step is with embodiment 1.
The above only is preferred embodiment of the present invention, is not to be the restriction of the present invention being made other form, and any those skilled in the art may utilize the technology contents of above-mentioned announcement to be changed or be modified as the equivalent embodiment of equivalent variations.But every technical solution of the present invention content that do not break away to any simple modification, equivalent variations and remodeling that above embodiment did, still belongs to the protection domain of technical solution of the present invention according to technical spirit of the present invention.
Claims (3)
1. the method for fucoidin is extracted in main laminaria comprehensive utilization, it is characterized in that utilizing the waste that produces in the process of sea-tangle for raw material production algin, iodine, N.F,USP MANNITOL to produce fucoidin, and this preparation method comprises the following order step:
(1). the pickles operation, take the mode of twice cover bubble to soak the sea-tangle that cuts through overdrying with 8-10 times of tap water, so that leach more iodine, N.F,USP MANNITOL, fucoidin in the water, the first pass of every batch of sea-tangle soaks water, enters cleaning section; Soak the first pass water that water is used to do the next batch dish for two times and carry out pickles; Sea-tangle is used to extract algin, and in the described pickles operation, behind the input sea-tangle, stirring replaces at least once with Jing Pao when soaking at every turn, stirs 0.5-3 minute; Quiet bubble 15-45 minute;
(2). cleaning section, the inorganic water conditioner of adding forms insolubles after soaking depositing in water to fall separation, adds flocculation agent with the intensive throw out of insolubles flocculation formation, carries out rough purification, removal of impurities, emits clear liquid to the alkali refining jar, and residue is drained;
Described inorganic water conditioner adopts at least a in bodied ferric sulfate, ferrous sulfate, Tai-Ace S 150, polymerize aluminum chloride, the poly-ferric chloride, working concentration is 100-150ppm, flocculation agent is conventional polyacrylamide macromolecular compound, and working concentration is 5-10ppm;
(3). clear liquid is emitted clear liquid and is used to extract iodine and N.F,USP MANNITOL in alkali refining jar alkali refining flocculation separation Fucose glue scum silica frost, and scum silica frost is retracted to retort with vacuum;
(4). the carbohydrate gum scum silica frost is adjusted the dissolving of pH value, adopt hydrochloric acid to regulate pH value 4-5, and heat to boil and carry, heat 75-90 ℃;
(5). the leach cooking liquid natural subsidence to layering, is discarded precipitation, supernatant liquor is filtered to see-through 〉=30cm with flocculating aids;
(6). the filtered liquid vacuum concentration, 3～5 times of described filtered liquid vacuum concentration make the concentrated solution solid content reach 40～50%, cooling, crystallization, separation desalination and N.F,USP MANNITOL;
(7). it is 25%-30% that above-mentioned clear liquid adds ethanol to alcohol concn, and natural subsidence discards precipitated impurities to layering behind the mixing;
(8). clear liquid is transferred pH value 1-3, acid degradation;
(9). with adding ethanol to alcohol concn in the degradation solution is 65-80%, and mixing, alcohol are analysed;
(10). natural subsidence and centrifugal the combining of machinery, alcohol analysed thing separates and washing with alcohol;
(11). the dry alcohol of sudden strain of a muscle formula is analysed thing, pulverizes and promptly gets the fucoidin product.
2. the method for claim 1 is characterized in that described clear liquid alkali refining uses caustic soda or white lime.
3. the method for claim 1 is characterized in that described flocculating aids is diatomite or perlite.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100689683A CN100425622C (en) | 2006-09-28 | 2006-09-28 | Method for extracting fucoidin by comprehensively utilizing kelp |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100689683A CN100425622C (en) | 2006-09-28 | 2006-09-28 | Method for extracting fucoidin by comprehensively utilizing kelp |
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| CN100540568C (en) * | 2007-04-20 | 2009-09-16 | 中国科学院海洋研究所 | A kind of method of extracting algal polysaccharide sulfate |
| CN101168570B (en) * | 2007-11-15 | 2010-05-26 | 暨南大学 | Method for degrading kelp polysaccharide sulfate |
| CN101156664B (en) * | 2007-11-21 | 2010-08-11 | 上海理工大学 | Method for distilling fucoidin from sea tangle caustic refining liquid |
| CN101830996B (en) * | 2010-04-21 | 2012-01-04 | 江南大学 | Method for separating and purifying blue algae polysaccharide |
| CN102173490B (en) * | 2011-03-07 | 2012-07-25 | 天津港源生物制品集团有限公司 | Flocculant formula used for stevioside extracting solution and use method thereof |
| CN102690367B (en) * | 2012-06-28 | 2013-11-20 | 合肥工业大学 | Preparation method of anti-atherosclerosis active laminarins |
| CN104945535B (en) * | 2013-04-22 | 2017-04-12 | 青岛贝尔特生物科技有限公司 | Method for production of sodium alginate and co-production of ethanol and seaweed organic fertilizer |
| CN104311698B (en) * | 2014-11-03 | 2016-08-24 | 青岛海百合生物技术有限公司 | A kind of Macrocystis pyrifera (L.) Ag. deep working method |
| CN106046188B (en) * | 2016-07-04 | 2018-12-21 | 青岛吉海营养科技有限公司 | A kind of preparation method of fucoidin |
| CN110511291A (en) * | 2019-08-27 | 2019-11-29 | 青岛明月海藻集团有限公司 | A kind of fast qualitative compares the method for fucoidin content in seaweed raw material |
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