CN113004434A - Sodium alginate degradation method based on bismuth tungstate photocatalyst - Google Patents
Sodium alginate degradation method based on bismuth tungstate photocatalyst Download PDFInfo
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- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 235000010413 sodium alginate Nutrition 0.000 title claims abstract description 54
- 229940005550 sodium alginate Drugs 0.000 title claims abstract description 54
- 239000000661 sodium alginate Substances 0.000 title claims abstract description 54
- 230000015556 catabolic process Effects 0.000 title claims abstract description 44
- 238000006731 degradation reaction Methods 0.000 title claims abstract description 44
- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 34
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 34
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 26
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 20
- 238000003756 stirring Methods 0.000 claims abstract description 15
- 239000003054 catalyst Substances 0.000 claims abstract description 8
- 239000002245 particle Substances 0.000 claims abstract description 8
- 239000006228 supernatant Substances 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 9
- 239000002244 precipitate Substances 0.000 claims description 8
- 229910020350 Na2WO4 Inorganic materials 0.000 claims description 5
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000005286 illumination Methods 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 229910052724 xenon Inorganic materials 0.000 claims description 3
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 8
- 230000003197 catalytic effect Effects 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 5
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- 230000000593 degrading effect Effects 0.000 abstract description 2
- 230000008961 swelling Effects 0.000 abstract 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical group O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 150000004676 glycans Chemical class 0.000 description 3
- 229920001282 polysaccharide Polymers 0.000 description 3
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- 230000005855 radiation Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000000725 suspension Substances 0.000 description 3
- 239000004408 titanium dioxide Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
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- 238000004458 analytical method Methods 0.000 description 2
- 239000008280 blood Substances 0.000 description 2
- 210000004369 blood Anatomy 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 description 1
- 239000005695 Ammonium acetate Substances 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 229920002307 Dextran Polymers 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 235000010443 alginic acid Nutrition 0.000 description 1
- 229920000615 alginic acid Polymers 0.000 description 1
- 229940043376 ammonium acetate Drugs 0.000 description 1
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- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006065 biodegradation reaction Methods 0.000 description 1
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- 239000002537 cosmetic Substances 0.000 description 1
- AEMOLEFTQBMNLQ-YBSDWZGDSA-N d-mannuronic acid Chemical compound O[C@@H]1O[C@@H](C(O)=O)[C@H](O)[C@@H](O)[C@H]1O AEMOLEFTQBMNLQ-YBSDWZGDSA-N 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 235000013376 functional food Nutrition 0.000 description 1
- 238000004192 high performance gel permeation chromatography Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
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- 239000004570 mortar (masonry) Substances 0.000 description 1
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- 210000005036 nerve Anatomy 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 238000001782 photodegradation Methods 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
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Images
Classifications
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/31—Chromium, molybdenum or tungsten combined with bismuth
-
- B01J35/39—
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
Abstract
The invention provides a bismuth tungstate photocatalyst with a molecular formula of Bi2WO6The diameter of the particles is 1-100nm, and the particles are cotton-shaped; the method for degrading sodium alginate by using the bismuth tungstate photocatalyst comprises the following steps: s1, preparing 0.01-2g/L sodium alginate solution, and fully swelling; s2, following a 100ml sodium alginate solution: adding 0.01-1g of bismuth tungstate into the solution as a photoreaction catalyst, and stirring the solution to uniformly distribute the catalyst in the solution; s3, stirring while illuminating; s4, centrifuging to obtain supernatant which is degraded sodium alginate solution. The method is environment-friendly, pollution-free, simple and convenient to operate, easy to obtain reaction conditions, free of special equipment requirements and low in production cost; book (I)The bismuth tungstate prepared by the method has the advantages of wide photoresponse range to a visible near-infrared light region, good visible light catalytic performance and the like, and the flocculent nano-scale bismuth tungstate has large specific surface area and is more favorable for catalytic degradation.
Description
Technical Field
The invention relates to the technical field of polysaccharide degradation, in particular to a method for obtaining low-molecular-weight sodium alginate by photo-degradation by using bismuth tungstate as a photocatalyst.
Background
Sodium alginate is a common form of algin, which is a linear polysaccharide mainly polymerized from α -L mannuronic acid (M) and β -D guluronic acid (G) through α -1,4 glycosidic linkages. China is the largest sodium alginate producing country in the world, and the production capacity exceeds 70% of the total production capacity. Sodium alginate has good stability and safety, and can be widely used in food industry and medicine field. However, sodium alginate is a polysaccharide substance with high polymerization degree, has the characteristics of strong gel property, high viscosity, poor water solubility, difficult absorption and the like, and limits the application of sodium alginate in the fields of biological medicines and the like.
The low molecular weight sodium alginate has the characteristics of strong water solubility, easy absorption and the like, and experiments and clinics find that the low molecular weight sodium alginate has biological activities of resisting oxidation, preventing freezing, preserving water, resisting tumors, inhibiting bacteria, regulating blood pressure, reducing blood fat, reducing blood sugar, protecting nerves and the like, and has wide development and application prospects in the fields of functional food, medicine development, green agriculture, cosmetic preparation and the like.
The existing method for preparing the low molecular weight sodium alginate mainly comprises chemical degradation, biological degradation and physical degradation. The acid degradation is a simple and common chemical method for degrading sodium alginate, but the reaction is violent, equipment corrosion is easily caused, and more waste liquid is generated; the biodegradation mainly comprises enzyme catalysis degradation, and the enzymolysis method has mild reaction conditions, strong specificity and high cost; the physical degradation is mainly ultrasonic degradation, microwave degradation and radiation degradation, but the equipment cost is higher.
The photocatalytic degradation refers to the degradation of target organic matters by utilizing radiation and free radicals generated by a photocatalyst in a reaction solution system. The degradation method is clean, utilizes solar energy, has no pollution to the environment, and has simple operation and low production cost. The most commonly used photocatalyst is titanium dioxide, but titanium dioxide can only generate electron-hole pairs under the excitation of ultraviolet rays with the wavelength of less than 380nm and then is converted into free radicals for degradation. In order to improve the degradation efficiency, the light response range of the photocatalyst is expanded from the viewpoint of utilizing solar energy; and bismuth tungstate can absorb sunlight below 450nm, and has the advantages of high stability, nano structure, high catalytic performance and the like. Therefore, the invention discloses a method for obtaining the low-molecular-weight sodium alginate by using the bismuth tungstate as the photocatalyst and utilizing the sunlight degradation.
Disclosure of Invention
The invention provides a method for obtaining low-molecular-weight sodium alginate by using bismuth tungstate as a photocatalyst and utilizing sunlight degradation, which aims to solve the problems of high cost, high equipment requirement, low degradation rate, environmental pollution and the like of the existing degradation method.
In order to realize the purpose, the invention provides a bismuth tungstate photocatalyst with a molecular formula of Bi2WO6The diameter of the particles is 1-100nm, and the particles are flocculent.
A sodium alginate degradation method of the bismuth tungstate photocatalyst comprises the following steps:
s1, preparing a 0.01-2g/L sodium alginate solution, and standing the prepared sodium alginate aqueous solution for 12-24h to fully swell the sodium alginate aqueous solution;
s2, according to the ratio of sodium alginate solution per 100 ml: adding 0.01-1g of bismuth tungstate into the solution as a photoreaction catalyst, and stirring the solution to uniformly distribute the catalyst in the solution;
s3, stirring for 2-10h while illuminating;
s4, stopping stirring, and centrifuging at the rotating speed of 4000-10000rpm to obtain a supernatant which is the degraded sodium alginate solution.
Preferably, the illumination light source in step S3 includes a 300-700w xenon lamp, and the distance from the sodium alginate solution is 1-10 cm.
A preparation method of the bismuth tungstate photocatalyst comprises the following steps:
s1, preparing equal volume of Bi (NO) with the concentration of 2.0-3.0mmol/L3)3·5H21M HNO of O3The solution and 1.0-1.5mmol of Na2WO4·2H2An aqueous solution of O;
s2, mixing Na2WO4·2H2Dripping Bi (NO) into the O solution at a speed of 1 drop in 2-5 seconds3)3·5H2In the O solution, and adjusting the pH value to 5-6 to obtain white precipitate;
s3, heating and stirring for 140min at a constant temperature water bath of 70-100 ℃ for 100-2WO6And (3) powder.
Preferably, the method for adjusting the pH in step S2 includes adding NaOH.
The invention has the beneficial effects that:
the method adopts a photocatalysis method to degrade sodium alginate, adds the photocatalyst bismuth tungstate, utilizes sunlight to degrade the sodium alginate, and has the advantages of environmental protection, low equipment requirement, simple reaction condition, simple and convenient operation, easy recovery of the photocatalyst and the like.
Compared with the existing methods such as an acid degradation method, an enzymolysis method, ultrasonic degradation, microwave degradation and radiation degradation, the method provided by the invention has the advantages of environmental friendliness, no pollution, simplicity and convenience in operation, easiness in obtaining of reaction conditions, no need of special equipment requirements and low production cost.
Compared with common photocatalyst titanium dioxide, the bismuth tungstate used in the invention has the advantages of wide photoresponse range to a visible near-infrared light region, good visible light catalytic performance and the like. And the cotton-shaped nano bismuth tungstate has larger specific surface area, and is more favorable for catalytic degradation.
Drawings
FIG. 1 is a graph of X-ray diffraction (top) against a standard card (bottom) of bismuth tungstate prepared in accordance with the present invention;
FIG. 2 is a scanning electron microscope image of bismuth tungstate prepared by the invention;
FIG. 3 is a high performance gel permeation chromatogram of sodium alginate in accordance with the present invention;
FIG. 4 is a high performance gel permeation chromatogram of sodium alginate degradation of the invention for 0 hour;
FIG. 5 is a high performance gel permeation chromatogram of sodium alginate degradation of the present invention for 1 hour;
FIG. 6 is a high performance gel permeation chromatogram of sodium alginate degradation of the present invention for 2 hours;
FIG. 7 is a high performance gel permeation chromatogram of sodium alginate degradation of the present invention for 3 hours;
FIG. 8 is a high performance gel permeation chromatogram of sodium alginate degradation of the present invention for 4 hours;
FIG. 9 is a high performance gel permeation chromatogram of sodium alginate degradation of the present invention for 5 hours;
FIG. 10 is a high performance gel permeation chromatogram of sodium alginate degradation of the present invention for 6 hours.
Detailed Description
Example 1: preparation of bismuth tungstate
Preparing Bi (NO) with concentration of 2.5mmol/L by coprecipitation method3)3·5H21M HNO of O350ml of the solution was dissolved by magnetic stirring at room temperature to obtain solution A. The solution was prepared to contain 1.25mmol of Na2WO4·2H250ml of an aqueous solution of O to obtain a solution B. Then slowly dripping the solution B (1 drop in 2-5 seconds) into the solution A, andadjusting the pH value of the mixed solution to 5.5 by using NaOH solution to obtain white precipitate, heating and stirring the white precipitate in 80 ℃ constant temperature water bath for 120min, centrifuging the obtained suspension for 5min at 5000rpm, alternately cleaning the white precipitate by using deionized water and absolute ethyl alcohol for 3 times, drying the white precipitate in a drying oven at 80 ℃, grinding the white precipitate in an agate mortar, calcining the dried suspension in a 600 ℃ muffle furnace for 4h, and grinding the dried suspension again to obtain Bi2WO6And (3) powder.
As shown in FIG. 1, Bi is prepared2WO6And (4) carrying out X-ray diffraction (XDR) analysis to obtain a characteristic diffraction peak of the sample, and comparing the characteristic diffraction peak with a standard card. As shown in FIG. 2, Bi is prepared2WO6Performing electron and Scanning Electron Microscope (SEM) analysis, and shooting the microscopic morphology of the obtained bismuth tungstate at 1 mu m and 100 nm; the diameter of the prepared bismuth tungstate particles is about 80nm, and the bismuth tungstate particles are flocculent. Compared with the sheet-packed bismuth tungstate produced in the prior art, the flocculent bismuth tungstate can further enlarge the surface area, is easier to contact with reaction substances, and is more favorable for catalytic degradation.
Example 2: degradation sodium alginate
Preparing 1g/L sodium alginate solution, weighing 1g of sodium alginate into a beaker, adding 1000ml of deionized water, stirring until the sodium alginate is completely dissolved in water, and standing the prepared sodium alginate aqueous solution for 12 hours to fully swell the sodium alginate aqueous solution. Measuring 200ml of 1g/L sodium alginate solution in a beaker, adding 0.2g of bismuth tungstate serving as a photoreaction catalyst, and stirring to ensure that the catalyst is uniformly distributed in the solution as much as possible. A500 w xenon lamp is adopted to simulate the irradiation of sunlight, the distance between the lamp and the sample is 5cm, and the stirring is carried out for 6 hours while the illumination is carried out. And respectively taking 1.5ml of reaction liquid to be tested when the photocatalytic reaction is carried out for 0h, 1h, 2h, 3h, 4h, 5h and 6 h. And stopping stirring when the reaction is finished, centrifuging (4000rpm) for 10min, wherein the supernatant is a degraded sodium alginate solution, the precipitate obtained by centrifuging is bismuth tungstate, and the bismuth tungstate can be recycled.
Centrifuging the sample at 8000rpm for 10min, collecting supernatant, and passing through 0.22 μm water system membrane. The relative molecular mass (Mw) was determined by high performance gel permeation chromatography using a TSK-gel G4000PWxl (7.5 mm. times.30.0 cm) column, a differential refractometer, and a column box temperature of 30 ℃. The mobile phase was ammonium acetate buffer (0.1mol/L, pH 6.0) at a flow rate of 0.4 mL/min. Dextran (relative molecular mass of 5, 12, 25, 50, 150, 410 and 670kDa, respectively) was used as standard. And (3) calculating the molecular weight of the sodium alginate after photocatalytic degradation by taking the retention time tR of the chromatographic peak as an abscissa and the lg Mw as an ordinate as a standard curve. As shown in FIG. 3, the original molecular weight of sodium alginate used in the experiment is 78kDa, and the molecular weight is 59kDa after 3 hours of degradation and is reduced to 40kDa after 6 hours of degradation as the degradation time is prolonged. FIGS. 4-10 show the relative molecular weight of sodium alginate after degradation for 0-6h, wherein the relative molecular weight reaches 59kDa after 3h degradation, the molecular weight is reduced to 40kDa after 6h degradation, and the degradation effect is very obvious.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be able to cover the technical solutions and the inventive concepts of the present invention within the technical scope of the present invention.
Claims (5)
1. The bismuth tungstate photocatalyst is characterized in that the molecular formula is Bi2WO6The diameter of the particles is 1-100nm, and the particles are flocculent.
2. A sodium alginate degradation method based on the bismuth tungstate photocatalyst in claim 1 is characterized by comprising the following steps:
s1, preparing a 0.01-2g/L sodium alginate solution, and standing the prepared sodium alginate aqueous solution for 12-24h to fully swell the sodium alginate aqueous solution;
s2, according to the ratio of sodium alginate solution per 100 ml: adding 0.01-1g of bismuth tungstate into the solution as a photoreaction catalyst, and stirring the solution to uniformly distribute the catalyst in the solution;
s3, stirring for 2-10h while illuminating;
s4, stopping stirring, and centrifuging at the rotating speed of 4000-10000rpm to obtain a supernatant which is the degraded sodium alginate solution.
3. The sodium alginate degradation method as claimed in claim 2, wherein the illumination light source in step S3 comprises a 300-700w xenon lamp, and the distance from the sodium alginate solution is 1-10 cm.
4. A preparation method of the bismuth tungstate photocatalyst as described in claim 1, which is characterized by comprising the following steps:
s1, preparing equal volume of Bi (NO) with the concentration of 2.0-3.0mmol/L3)3·5H2HNO of O3The solution and 1.0-1.5mmol of Na2WO4·2H2An aqueous solution of O;
s2, mixing Na2WO4·2H2Dripping Bi (NO) into the O solution at a speed of 1 drop in 2-5 seconds3)3·5H2In the O solution, and adjusting the pH value to 5-6 to obtain white precipitate;
s3, heating and stirring for 140min at a constant temperature water bath of 70-100 ℃ for 100-2WO6And (3) powder.
5. The method of preparing a bismuth tungstate photocatalyst as claimed in claim 4, wherein the method of adjusting the pH in step S2 includes adding NaOH.
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