CN101125893A - Method for preparing high-purity fucoidin from slag and liquid of sea-tangle chemical industry production - Google Patents
Method for preparing high-purity fucoidin from slag and liquid of sea-tangle chemical industry production Download PDFInfo
- Publication number
- CN101125893A CN101125893A CNA2006100690591A CN200610069059A CN101125893A CN 101125893 A CN101125893 A CN 101125893A CN A2006100690591 A CNA2006100690591 A CN A2006100690591A CN 200610069059 A CN200610069059 A CN 200610069059A CN 101125893 A CN101125893 A CN 101125893A
- Authority
- CN
- China
- Prior art keywords
- fucoidin
- electrodialysis
- liquid
- fucokinase
- sea
- 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.)
- Pending
Links
Landscapes
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a method of preparing high purity fucokinase by residue and liquid produced by sea tangle chemical engineering. The invention is characterized in that sea tangle steepwater, vegetable-washing water, sea tangle floating residue liquid and formaldehyde washing water are preprocessed to obtain supernatant fluid, then the supernatant fluid is treated by levels with ethyl alcohol and dried, thus gaining fucokinase crude; the fucokinase crude solution is fed in electrodialysis cell to get fucokinase electrodialysis solution through electrodialysis, to which the ethyl alcohol is added to filter, thereby obtaining fucokinase electrodialysis purifying products; 10,000 to 100,000 fibral coats are chosen to trap coat of fucokinase liquid, then the concentration solution can be obtained after coat separation, to which the ethyl alcohol is added to filter, dehydrate and dry, thus obtaining fucokinase purifying products. The high purity of fucokinase is up to 35 to 40 percent, thereby solveing the quality and environmental pollution of iodine, alcohol and alginate influenced by the existing of fucokinase. The light brown product has various good indexes, properties, performances, and can be used as raw materials for depth developing products of fucokinase.
Description
Technical field
The present invention relates to the preparation of polyose, especially a kind of slag, liquid that utilizes sea-tangle chemical industry to produce prepares the method for high purity fucoidin.
Background technology
Sea-tangle chemical industry is the important algae secondary industry of China, is to be raw material with the sea-tangle, produces iodine, N.F,USP MANNITOL, algin three great tradition products.With algin production is example, and its production technique will be passed through kelp soaking → pre-treatment → digestion → analyse → decalcification → processes such as neutralization conversion → oven dry towards rare → floating → calcium.Dried sea-tangle with a large amount of water soak for a long time iodine and N.F,USP MANNITOL soak solution, will be in pretreatment process with the clear water repetitive scrubbing attached to the lip-deep viscous mass of frond, and after the sea-tangle employing formaldehyde immersion treatment, water washes the formaldehyde wash-down water that removes formaldehyde and produce; Digest in sea-tangle, in rare, floating operation, produce the floating slag liquid of a large amount of sea-tangles.Above-mentioned its main component of the viscous mass that rinses out is exactly a fucoidin, and it has very strong water absorbability with the humidity in the protection marine alga in frond, can stop marine alga to be exposed in the air dry and cracked in the time of low water.Simultaneously, the formaldehyde wash-down water also contains the fucoidin composition in the floating slag liquid of sea-tangle.Sea-tangle chemical industry enterprise does not carry out the recovery of fucoidin mostly at present, just is discharged as waste, has not only wasted valuable fucoidin resource but also had environmental pollution problem.
Fucoidin is a kind of water-soluble assorted poly-polysaccharide, it is the intercellular product of brown alga, its main component is the α-L-fucose polymer of sulfur-bearing acidic group, have preserve moisture, thickening, bacteriostatic action, enhancing body immunity, blood coagulation resisting function, reducing blood-fat, hypoglycemic, hypotensive activity, inhibition renal failure effect, anti HIV-1 virus effect, can be widely used in daily-use sanitary articles for use, makeup and healthcare products and field of medicaments.At present, Chinese scholars is devoted to extract the research of fucoidin and preparation low weight molecular fucoidan aspect mostly.But the fucoidin of extraction mostly is crude product.In the CN1229393C Chinese invention patent specification sheets that on November 30th, 2005 was announced a kind of microorganisms producing fucoidin enzyme that utilizes is disclosed for example, the technical scheme of utilizing the further hydrolysis of this enzyme to produce low weight molecular fucoidan, technology in this technical scheme comprises: be raw material with the brown alga, with raw material pulverizing, the back flooding of sieving, temperature is in the time of 40～100 ℃, stirring and leaching 6～10 hours, centrifugal removal solid substance, collect filtrate, concentrate, remove starch, ethanol precipitation, the throw out lyophilize obtains the fucoidin powder; Above-mentioned fucoidin is implemented enzyme digestion reaction; The back intensification that finishes makes enzyme forfeiture alive; Through the gel chromatography molecular sieving, lyophilize obtains low weight molecular fucoidan.Obtaining the fucoidin powder in this specification sheets mid-early stage technology also is the fucoidin crude product.Yet there are no the report that the slag, the liquid that utilize the sea-tangle chemical industry production process to produce prepare the high purity fucoidin.
Summary of the invention
For slag, the liquid that overcomes existing sea-tangle chemical industry production process generation is discharged as waste, the fucoidin of not only having wasted fucoidin resource but also contaminate environment and present disclosed extraction mostly is the problem of crude product, the invention provides the method that a kind of slag, liquid that utilizes sea-tangle chemical industry to produce prepares the high purity fucoidin, this method is to propose according to the production process route of sea-tangle chemical industry, not only solved because the existence of fucoidin, influence the quality and the problem of environmental pollution of iodine, alcohol, particularly algin, and the fucoidin purity height of preparation.
The technical scheme that technical solution problem of the present invention is adopted is: slag, the liquid that a kind of sea-tangle chemical industry produces prepares the method for high purity fucoidin, is characterized in: the following treatment process of process:
A, raw material are handled:
A.1 be raw material with kelp soaking water, vegetable washing water
It is 12 that kelp soaking water, vegetable washing water are adjusted pH value, and retrogradation was carried out precipitate and separate behind the resulting throw out thin up in 8 hours, got its supernatant liquor, and is standby;
A.2 be raw material with floating slag
After floating slag liquid adjusted the pH value and be 2-3, wash floatingly, after the solid-liquid separation, get its supernatant liquor, standby;
A.3 be raw material with the formaldehyde wash-down water
It is 2-3 that the formaldehyde wash-down water is adjusted the pH value, carry out solid-liquid separation after, get its supernatant liquor, standby;
The preparation of b, fucoidin crude product
Merge supernatant liquors or three kinds of making are gone up the clear amalgamation liquids of liquid with any two kinds in above-mentioned three kinds of supernatant liquors that a.1, a.2, a.3 make any supernatant liquor in the step or make, add ethanol to 30% precipitation process, the filtering throw out, get its supernatant liquor and add ethanol to 70%, make throw out, after the dehydrated alcohol dehydration, be drying to obtain the fucoidin crude product; The product yield is at 0.6-2.8%, and the content of fucoidin is at 6-23%.
The electrodialysis purifying of c, fucoidin crude product
The fucoidin crude product that makes is dissolved in the fucoidin crude product solution that water makes 2.0-5.0%, this solution is inserted in the electrodialysis cell, do supporting electrolyte, control current density 0.020-0.080A/cm with NaCL solution
2, purifying 50-120 minute, get fucoidin electrodialysis solution, this solution 70% ethanol sedimentation gets fucoidin electrodialysis purifying product; The yield of this fucoidin is at 1-3%, and fucoidin content (%) is at 20-30%.The fucoidin electrodialysis solution of gained also can be directly as the raw material of next step membrane sepn.
For reducing overvoltage, the destruction that prevents fucoidin, the anode employing activating oxide coated anode of this electrodialysis cell, negative electrode employing metallic titanium plate negative electrode.
The membrane separation purification of the fucoidin behind d, the electrodialysis purifying
With the water-soluble fucoidin feed liquid that makes of the fucoidin purifying product after gained fucoidin electrodialysis solution or the electrodialysis process after the above-mentioned electrodialysis process, select for use the bear electricity cellulose acetate film of 1-10 ten thousand to make mwco membrane, under the magnetic agitation condition, adopt suitable operating pressure, behind membrane sepn, obtain concentrated solution, add ethanol to 70%, generate throw out, this throw out ethanol dehydration, the dry high purity fucoidin that gets.The yield of this fucoidin is at 1-3%, and fucoidin content (%) is at 30-40%.
Kelp soaking water, vegetable washing water or floating slag liquid or formaldehyde wash-down water that the present invention adopts the production process route of sea-tangle chemical industry to make make supernatant liquor through handling, make the fucoidin crude product through the alcohol grading processing, again the fucoidin crude product is handled through electrodialysis purifying, membrane sepn, make fucoidin purifying product, this fucoidin purity height, reach 35-40%, also solved existence simultaneously, influence the quality and the problem of environmental pollution of iodine, alcohol, particularly algin owing to fucoidin.It is light brown that product is, and every index, proterties, performance and outward appearance are all good, can be used as the raw material of fucoidin deep development product.
Embodiment
The present invention will be further described below in conjunction with embodiment.
The immersion water, vegetable washing water, floating slag and the formaldehyde wash-down water that produce with the sea-tangle chemical industry production process are the process explanation preparation method of the present invention that point of penetration and raw material extract fucoidin.
Example 1
With kelp soaking water is raw material, regulating pH value with sodium hydroxide solution is 12, the throw out that retrogradation obtained in 8 hours carries out precipitate and separate again behind the thin up, get supernatant liquor and add ethanol to 30%, separating obtained throw out enters the algin production line, get its supernatant liquor and continue to add ethanol to 70%, the throw out of generation is after the dehydrated alcohol dehydration, be drying to obtain thick fucoidin, its fucoidin content is 17.8%; The thick fucoidin solution of preparation 2.5% is inserted in the electrodialysis cell, for reducing overvoltage, the destruction that prevents fucoidin, the anode employing activating oxide coated anode of this electrodialysis cell, negative electrode employing metallic titanium plate negative electrode, control current density 0.060A/cm
2, purifying 80 minutes only produces a small amount of CL
2, do not have colloid flocculation substantially, ion-exchange membrane does not stop up, fucoidin is given birth to matter does not have bad variation, under 70% ethanol condition, precipitate fucoidin electrodialysis purifying product, yield is at 1-3%, its fucoidin content is 23%; With the water-soluble fucoidin feed liquid that makes of the fucoidin purifying product after the electrodialysis process, select for use 50,000 molecular weight throttling films to make mwco membrane, under the magnetic agitation condition, adopt suitable operating pressure, behind membrane sepn, obtain concentrated solution, add ethanol to 70%, produce throw out, this throw out ethanol dehydration, the dry high purity fucoidin that gets.Its fucoidin content can reach 34.3%.
Example 2
With the formaldehyde wash-down water is raw material, elder generation's adjust pH is 2-3, carry out solid-liquid separation, its supernatant liquor adds ethanol to 30%, throw out mainly is an algin, gets its supernatant liquor and continues to add ethanol to 70%, after the throw out of generation dewaters with dehydrated alcohol, be drying to obtain thick fucoidin, its product fucoidin content is 18.4%.The thick fucoidin solution of preparation 3.5% is inserted in the electrodialysis cell, and the anode of this electrodialysis cell adopts the activating oxide coated anode, and negative electrode adopts metallic titanium plate, control current density 0.080A/cm
2, purifying 100 minutes gets fucoidin electrodialysis solution; Be somebody's turn to do to such an extent that fucoidin electrodialysis solution also can be used 70% ethanol sedimentation, get the electrodialysis purifying product of fucoidin, its fucoidin content can reach 26.0%; Fucoidin electrodialysis solution with preparation, select for use 10,000 molecular weight throttling films to be further purified as mwco membrane, under the magnetic agitation condition, adopt suitable operating pressure, behind membrane sepn, obtain concentrated solution, add ethanol to 70%, produce throw out, this throw out ethanol dehydration, the dry high purity fucoidin that gets.Its fucoidin content reaches 31.2%.
The immersion water that the present invention makes according to the sea-tangle chemical industry production process, vegetable washing water or floating or formaldehyde wash-down water prepare the fucoidin crude product, make highly purified fucoidin through electrodialysis purifying, membrane separation purification again.The product yield is at 1-3%, and fucoidin content (%) is at 30-40%.
Claims (5)
1. slag, the liquid of a sea-tangle chemical industry generation prepare the method for high purity fucoidin, it is characterized in that: the following treatment process of process:
A, raw material are handled:
A.1 be raw material with kelp soaking water, vegetable washing water
It is 12 that kelp soaking water, vegetable washing water are adjusted pH value, and retrogradation was carried out precipitate and separate behind the resulting throw out thin up in 8 hours, got its supernatant liquor, and is standby;
A.2 be raw material with floating slag
After floating slag liquid adjusted the pH value and be 2-3, wash floatingly, after the solid-liquid separation, get its supernatant liquor, standby;
A.3 be raw material with the formaldehyde wash-down water
It is 2-3 that the formaldehyde wash-down water is adjusted the pH value, carry out solid-liquid separation after, get its supernatant liquor, standby;
The preparation of b, fucoidin crude product
Merge supernatant liquors or three kinds of making are gone up the clear amalgamation liquids of liquid with any two kinds in above-mentioned three kinds of supernatant liquors that a.1, a.2, a.3 make any supernatant liquor in the step or make, add ethanol to 30% precipitation process, the filtering throw out, get its supernatant liquor and add ethanol to 70%, make throw out, after the dehydrated alcohol dehydration, be drying to obtain the fucoidin crude product;
The electrodialysis purifying of c, fucoidin crude product
The fucoidin crude product that makes is dissolved in the fucoidin crude product solution that water makes 2.0-5.0%, this solution is inserted in the electrodialysis cell, do supporting electrolyte, control current density 0.020-0.080A/cm with NaCL solution
2, purifying 50-120 minute, get fucoidin electrodialysis solution, this solution 70% ethanol sedimentation gets fucoidin electrodialysis purifying product;
The membrane separation purification of the fucoidin behind d, the electrodialysis purifying
With the water-soluble fucoidin feed liquid that makes of the fucoidin purifying product after gained fucoidin electrodialysis solution or the electrodialysis process after the above-mentioned electrodialysis process, select for use the bear electricity cellulose acetate film of 1-10 ten thousand to make mwco membrane, under the magnetic agitation condition, adopt suitable operating pressure, behind membrane sepn, obtain concentrated solution, add ethanol to 70%, generate throw out, this throw out ethanol dehydration, the dry high purity fucoidin that gets.
2. slag, the liquid that a kind of sea-tangle chemical industry according to claim 1 produces prepares the method for high purity fucoidin, it is characterized in that: the anode of described electrodialysis cell adopts the activating oxide coated anode, and negative electrode adopts the metallic titanium plate negative electrode.
3. slag, the liquid that a kind of sea-tangle chemical industry according to claim 1 produces prepares the method for high purity fucoidin, and it is characterized in that: the yield of described fucoidin crude product is at 0.6-2.8%, and the content of fucoidin is at 6-23%.
4. slag, the liquid that a kind of sea-tangle chemical industry according to claim 1 and 2 produces prepares the method for high purity fucoidin, and it is characterized in that: the yield of described fucoidin electrodialysis purifying product is at 1-3%, and fucoidin content (%) is at 20-30%.
5. slag, the liquid that a kind of sea-tangle chemical industry according to claim 1 and 2 produces prepares the method for high purity fucoidin, and it is characterized in that: the yield of the membrane separation purification of described fucoidin is at 1-3%, and fucoidin content (%) is at 30-40%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2006100690591A CN101125893A (en) | 2006-09-21 | 2006-09-21 | Method for preparing high-purity fucoidin from slag and liquid of sea-tangle chemical industry production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2006100690591A CN101125893A (en) | 2006-09-21 | 2006-09-21 | Method for preparing high-purity fucoidin from slag and liquid of sea-tangle chemical industry production |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101125893A true CN101125893A (en) | 2008-02-20 |
Family
ID=39094042
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2006100690591A Pending CN101125893A (en) | 2006-09-21 | 2006-09-21 | Method for preparing high-purity fucoidin from slag and liquid of sea-tangle chemical industry production |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101125893A (en) |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891838A (en) * | 2010-07-29 | 2010-11-24 | 中国水产科学研究院黄海水产研究所 | Method for recovering residual algin from floating waste residue liquid in seaweed chemical production |
| CN101813593B (en) * | 2009-02-23 | 2011-06-08 | 中国水产科学研究院东海水产研究所 | Method for detecting purity of sodium alginate |
| CN102471385A (en) * | 2009-07-28 | 2012-05-23 | Cp凯可股份公司 | Dewatering biomass material comprising polysaccharide, method for extracting polysaccharide from biomass material, and dewatered biomass material |
| CN102827301A (en) * | 2012-09-06 | 2012-12-19 | 大连海洋大学 | Method for separating and purifying fucosan sulfate by salt deposition combined with electrodialysis |
| CN103788219A (en) * | 2012-10-30 | 2014-05-14 | 中国科学院海洋研究所 | Method for extracting and preparing low molecular fucoidan from Ascophyllum mackaii |
| CN106008737A (en) * | 2016-07-14 | 2016-10-12 | 大连工业大学 | Sporophyl polysaccharides of undaria pinnatifida and preparation method for sporophyl polysaccharides |
| CN106046188A (en) * | 2016-07-04 | 2016-10-26 | 青岛吉海营养科技有限公司 | Method for preparing fucoidin |
| 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 |
| CN111548427A (en) * | 2019-02-12 | 2020-08-18 | 湖北洪森生物科技有限公司 | Preparation method of high-activity rice polysaccharide powder |
| CN111802653A (en) * | 2020-09-14 | 2020-10-23 | 烟台嘉惠海洋生物科技有限公司 | Tuna oligopeptide powder composition and preparation method and application thereof |
-
2006
- 2006-09-21 CN CNA2006100690591A patent/CN101125893A/en active Pending
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101813593B (en) * | 2009-02-23 | 2011-06-08 | 中国水产科学研究院东海水产研究所 | Method for detecting purity of sodium alginate |
| CN102471385A (en) * | 2009-07-28 | 2012-05-23 | Cp凯可股份公司 | Dewatering biomass material comprising polysaccharide, method for extracting polysaccharide from biomass material, and dewatered biomass material |
| CN101891838A (en) * | 2010-07-29 | 2010-11-24 | 中国水产科学研究院黄海水产研究所 | Method for recovering residual algin from floating waste residue liquid in seaweed chemical production |
| CN102827301B (en) * | 2012-09-06 | 2015-11-18 | 大连海洋大学 | Salt is heavy in conjunction with electrodialysis separation and purification fucoidan method |
| CN102827301A (en) * | 2012-09-06 | 2012-12-19 | 大连海洋大学 | Method for separating and purifying fucosan sulfate by salt deposition combined with electrodialysis |
| CN103788219B (en) * | 2012-10-30 | 2016-02-10 | 中国科学院海洋研究所 | A kind of extraction from bladder wrack prepares the method for low molecule fucoidan |
| CN103788219A (en) * | 2012-10-30 | 2014-05-14 | 中国科学院海洋研究所 | Method for extracting and preparing low molecular fucoidan from Ascophyllum mackaii |
| CN106046188A (en) * | 2016-07-04 | 2016-10-26 | 青岛吉海营养科技有限公司 | Method for preparing fucoidin |
| 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 |
| CN106008737A (en) * | 2016-07-14 | 2016-10-12 | 大连工业大学 | Sporophyl polysaccharides of undaria pinnatifida and preparation method for sporophyl polysaccharides |
| CN106008737B (en) * | 2016-07-14 | 2019-06-04 | 大连工业大学 | A kind of Undaria pinnatifida Suringar polysaccharide and preparation method thereof |
| 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 |
| CN111548427A (en) * | 2019-02-12 | 2020-08-18 | 湖北洪森生物科技有限公司 | Preparation method of high-activity rice polysaccharide powder |
| CN111802653A (en) * | 2020-09-14 | 2020-10-23 | 烟台嘉惠海洋生物科技有限公司 | Tuna oligopeptide powder composition and preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101125893A (en) | Method for preparing high-purity fucoidin from slag and liquid of sea-tangle chemical industry production | |
| US12006374B2 (en) | Nanocellulose compositions and processes to produce same | |
| Ji et al. | Enhancement of lignin removal and enzymolysis of sugarcane bagasse by ultrasound-assisted ethanol synergized deep eutectic solvent pretreatment | |
| Liu et al. | Synergism of organic acid and deep eutectic solvents pretreatment for the co-production of oligosaccharides and enhancing enzymatic saccharification | |
| Chang et al. | Comparison of sodium hydroxide and calcium hydroxide pretreatments on the enzymatic hydrolysis and lignin recovery of sugarcane bagasse | |
| US20030013871A1 (en) | Method of preparing modified cellulose ether | |
| EP3837246A2 (en) | Redox-active compounds and uses thereof | |
| WO2014092873A1 (en) | Processes and apparatus for lignin separation in biorefineries | |
| WO2015200584A1 (en) | Processes for producing nanocellulose-lignin composite materials, and compositions obtained therefrom | |
| JP2006238728A (en) | Method for producing sugars from drainage during papermaking | |
| CN106832036A (en) | The preparation method of algal polysaccharides extract | |
| CN106103726A (en) | Separate the method for oligosaccharides from agricultural wastes classification | |
| EP3219737A1 (en) | Ionic polymers and use thereof in processing of biomass | |
| CN101274947A (en) | Method for extracting lignosulphonate from sodium sulfite bamboo pulp waste liquor | |
| CN104232705A (en) | Method for pretreating lignocellulose at low temperature through coupling of sodium hydroxide and ethanol | |
| CN101168570B (en) | Method for degrading kelp polysaccharide sulfate | |
| CN110004756B (en) | Method for separating components of wood fiber biomass | |
| CN102417564B (en) | Water-retaining agent and preparation method thereof by papermaking sludge | |
| Rezania et al. | Changes in composition and structure of water hyacinth based on various pretreatment methods | |
| US20160326697A1 (en) | Refining cellulose in a solvent for production of nanocellulose materials | |
| CN106480129A (en) | A kind of preparation method of nano-cellulose | |
| CN115821619A (en) | Method for extracting lignin from sulfate pulping waste liquid | |
| WO2015187296A1 (en) | Refining cellulose in a solvent for production of nanocellulose materials | |
| KR20170004233A (en) | Method for preparing galactose using agarese | |
| KR101938200B1 (en) | Novel Method for Recovery of Xylose from Byproducts Generated in Biomass-Pretreatment Processes and Use Thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |