CN105771923A - Melamine sponge /alginic acid composite type adsorbing material and preparation method thereof - Google Patents
Melamine sponge /alginic acid composite type adsorbing material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a melamine sponge and alginic acid composite type adsorbing material and a preparation method thereof. The specific three-dimensional skeleton structure of a commercial melamine sponge is used, a sodium alginate aqueous solution is introduced and solidified in the sponge under an acid condition, then water in alginic acid is removed by a natural drying method, finally a unique three-dimensional macropore system is formed, wherein the melamine sponge has the effects of mechanical stabilization and supporting, the alginic acid is sufficiently dispersed to form a multilayer penetration shaped film, the adsorbing efficiency is obviously improved, the content of the alginic acid in the composite material is in the range of 52-58wt.%, and the specific surface area is in the range of 52.6-61.4m<2>/g.The composite type adsorbing material can be used as a whole adsorbing column, and can be used for extracting wine red natural pigments, and good effects are achieved. The material has the advantages that the absorbing capacity is high, the operation is simple and convenient, the material can be repeatedly recycled, the cost is reduced, and the production efficiency is improved.
Description
Technical field
The present invention relates to the polymer adsorbing material field for nature strength, especially a kind of melamine sponge and the compound adsorbing material of alginic acid and preparation method thereof, can be used to rapidly and efficiently extraction Fructus Vitis viniferae red natural coloring matter with it.
Background technology
Alginic acid, also known as alginic acid, alginic acid, seaweeds, is present in a kind of natural polysaccharide in Brown algae cell wall.Alginic acid (Alginicacid) is by the polysaccharide of monosaccharide aldehydic acid linear polymerization, monomer is β-D-manna aldehydic acid (M) and α-L-guluronic acid (G), M and G unit is with M-M, the compound mode of G-G or M-G passes through 1,4 glycosidic bonds are connected becomes block copolymer, and the empirical formula of alginic acid is (C6H8O6)n, molecular weight ranges is from 1 ten thousand to 60 ten thousand not etc..Alginic acid can quickly absorb moisture, papermaking and textile industry are used as dehydrant and sizing agent, its main function is that the form with sodium alginate or potassium salt is used as emulsifying agent or thickening agent in food industry and household chemicals industry, in pharmacy industry, alginic acid is conventional adjuvant, its viscosity makes it the binding agent of tablet, due to its water-swellable, it is used as again disintegrating agent and tablet is dispersed in human body, or be used as dispersant effective ingredient becomes suspension in liquid, alginate is often used as medicinal slow release agent, dentistry substitutes Gypsum Fibrosum and rubber with it, make tooth mould, alginic acid itself can treat heavy metal poisoning as absorbent.
Melamine sponge is a kind of expanded material formed by tripolycyanamide and formaldehyde condensation, there is the three dimensional skeletal structure that comparison is regular, through modified melamine sponge, also there is higher toughness, simple melamine sponge and alginic acid are difficult to use as adsorbing material, but both are combined cleverly and but can constitute a kind of brand-new large pore material, and utilize the characteristic of alginic acid natural polymer, can be used for the extraction of natural pigment.The present invention provides a kind of melamine sponge and the compound adsorbing material of alginic acid, its structure is as shown in Figure 1, melamine sponge provides three dimensional skeletal structure, itself there is the aperture of about 100 μm, can playing mechanically stable and supporting role, alginic acid then can form multilamellar penetration state thin film, and the thickness of thin film is at about 1 μm, three-dimensional framework and plural layers intert mutually, constitute three-dimensional big pore system.This composite construction not only increases the degree of scatter of alginic acid, thus improving its adsorption efficiency, the supporting role that melamine sponge provides simultaneously makes composite construction permeability good, liquid is made easily to flow in inside, thus composite can be used as monolithic devices absorption pillar, the invention provides application example, it was demonstrated that this material has extraordinary effect in the extraction to grape haematochrome.
Grape haematochrome is indispensable natural pigment in food industry, is extensively added in fruit wine, fruit jam, acidic beverages, improves the color and luster of product.
Summary of the invention
Primary technical problem to be solved by this invention is to provide a kind of melamine sponge/compound adsorbing material of alginic acid, and it can play an important role in the rapidly and efficiently extraction of grape haematochrome.
The preparation method that another technical problem to be solved by this invention is to provide above-mentioned melamine sponge/compound adsorbing material of alginic acid, it is practical, easy and simple to handle, it is easy to prepare in a large number.
Another technical problem to be solved by this invention is to provide the concrete application in grape haematochrome extracts of a kind of above-mentioned melamine sponge/compound adsorbing material of alginic acid.
1, this invention address that the technical scheme that primary technical problem adopts is: a kind of melamine sponge/chitosan composite adsorbing material, its structure has feature as shown in Figure 1, wherein alginic acid content is in 52～58wt.% scope, this material had both had the through duct of three-dimensional net structure and 100 μm, having again the multilamellar penetration state alginic acid thin film of about 1 μ m-thick, its specific surface area reaches 52.6～61.4m2/ g, adsorption efficiency is high, and liquid is easier at internal circulation, and can be easy to adsorbent eluting, it is achieved the repeatedly recycling of material.
Very usefully, alginic acid improves the adsorption efficiency of alginic acid on the one hand with melamine sponge compound, melamine sponge three-dimensional framework serves mechanically stable and supporting role on the other hand, make composite construction permeability good, liquid flowing quickly can be made, thus this composite can be used as globality absorption pillar, in nature strength process, significantly improve operating efficiency.
2, this invention address that the technical scheme that another technical problem adopts is: the preparation method of a kind of above-mentioned melamine sponge/compound adsorbing material of alginic acid, its characterization step is: (viscosity 200 ± 20mpa.s) soluble in water for the sodium alginate of commodity 1) is made into the concentration of 3～4wt.%, commercially available melamine sponge (tripolycyanamide and formaldehyde crosslinking react the foamed materials made, now commercialization) is immersed in the solution of thickness 1～2 hour；2) put into rapidly after taking out in the sulfuric acid solution of pH=3～4 and soak 2～3 hours, complex is put in clear water and rinse 4～5 hours under room temperature；3) being placed under room temperature by complex ventilation natural drying, after 3～4 days, inside compounds forms macroporous structure as shown in Figure 1.
Very usefully, sodium alginate soln is quick solidification in sour environment, it is transformed into alginic acid, process through room temperature natural drying, multilamellar penetration state pattern as shown in Figure 1 can be formed, and thin film keeps certain orientation in natural drying process, together with this pattern is interspersed in original three-dimensional framework, thus alginic acid can not bond agglomerating, thus keeping the specific surface area that it is bigger, after bi-material compound, its mechanical strength is higher, and anti-pressure ability is higher, entirely appropriate for monolithic devices adsorption column.
3, this invention address that the technical scheme that another technical problem adopts is: the above-mentioned melamine sponge/compound adsorbing material of alginic acid application process in glucose red pigment extracts, it is characterized in that being superimposed some blocks of column type materials, it is placed in a glass columns, constitute monolithic devices absorption pillar, material solution is infiltrated and flows through this material, extract is adsorbed on the skeleton of polymer, is collected by extract again through eluting, to reach the purpose of Separation & Purification.
Very usefully, above-mentioned processing method wants efficient quick than general direct mixing method, the problem being absent from diffusion hindered, find through overtesting, each gram of alginic acid can adsorb the grape haematochrome of 103～127 milligrams, and its absorbability is higher than the processing method that alginic acid directly mixes with material solution.
It is an advantage of the current invention that: 1) new adsorbing material aperture is big, is conducive to liquid to flow, and resistance is little；2) alginic acid forms thickness and is only the thin film of 1 μm, good dispersion, and specific surface area is big, improves the adsorption efficiency of alginic acid；3) composite construction good mechanical stability, anti-pressure ability is strong, thus can adsorb in monolithic devices pillar mode, and operating efficiency is high.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail.
Prepared by adsorbing material:
1) (viscosity 200 ± 20mpa.s) soluble in water for the sodium alginate of commodity is made into the concentration of 3～4wt.%, commercially available melamine sponge (tripolycyanamide and formaldehyde crosslinking react the foamed materials made, now commercialization) is immersed in the solution of thickness 1～2 hour；
2) complex is put into rapidly in the sulfuric acid solution of pH=3～4 and soak 2～3 hours, then complex is put in clear water and to rinse 4～5 hours under room temperature；
3) it is placed under room temperature by complex ventilation natural drying, after 3～4 days, inside compounds forms macroporous structure as shown in Figure 1, by 6 preparation experiments, with gravimetric detemination, in material, alginic acid accounts for 52～58wt.% scope, the change of alginic acid content comes from the variable density of melamine sponge and the small size change of sodium alginate soln concentration, measures the specific surface area of material at 52.6～61.4m with specific surface instrument2/ g range.
The extraction of grape haematochrome is undertaken by following operating procedure:
A. pretreatment, by broken for dry Radix seu Herba Tetrastigmatis Hypoglauci corium farinosum and cross 40 mesh sieves；
B. extracting, be placed in stainless-steel pan by the dry Radix seu Herba Tetrastigmatis Hypoglauci skin processed above, when stirring, add 5 times of weight 50% ethanol waters, 60 DEG C are stirred extraction 1～2 hour, collect by filtration filtrate；Filtering residue extracts once by the same method, combining extraction liquid；
C. concentrating, reduce pressure distillation and concentration by above-mentioned extract, reclaims ethanol, obtains pigment solution, and be filtered to remove residue；
D. separate, by above-mentioned pigment solution, by the integral post be made up of melamine sponge/compound adsorbing material of alginic acid, (diameter is 10cm, it is highly 100cm, it is formed by stacking by 5 pieces of cylindric samples), the volume of pigment solution should be 1: 1.5～1: 2.0 with the volume of pillar ratio with it, and remaining liquid, at 50～60mL/min, is finally extruded pillar with air by flow speed control, the liquid color flowed out substantially shoals, and the color of pillar becomes Fructus Vitis viniferae redness；
E. eluting, with the ethanol elution pillar of 95%, controls same flow velocity, until effluent does not have color, collects eluent, decompression distillation, reclaims ethanol, obtain pigment concentrate；
F. dry, by vacuum drying under pigment concentrate room temperature, obtain pigment powder.
Content analysis:
Take after 2.1% citric acid solution 159 points (volume) and 0.16% disodium phosphate soln 41 points (volumes) mix, adjust to pH3.0 with citric acid solution or disodium phosphate soln, this solution is standby as buffer solution, accurately weigh appropriate sample, so that the absorbance recorded is as the criterion between 0.2～0.7, it is settled to 100mL plus above-mentioned buffer solution, 1cm absorption cell measures its absorbance A being about 525nm place at maximum absorption wave, with above-mentioned buffer solution as blank assay, the chromatic value of sample calculates with equation below
Colourity=A × 10/ sample size (g)
The colourity testing obtained grape haematochrome is not less than FAO/WHO standard
Alkalescence colorimetric analysis:
Materials 1g, adds 5% sodium hydroxide solution 100mL, fully shakes up, and takes time solution 30mL, extracts with 15mL ether, and with spirit of vinegar back extraction ether extraction liquid twice, each 5mL, secondary acetic acid anti-stripping agent is colourless, illustrates not have in sample alkaline pigment.
Material absorbability is assessed:
The dry state density of melamine sponge/compound adsorbing material of alginic acid is generally 0.04～0.05g/mL, the volume of integral post is 7.85L, its quality is 314～393g, meansigma methods is 353g, calculate according to the meansigma methods 55% of alginic acid content, the gross weight of alginic acid is 194g, integral post is after fully absorption, through eluting, the amount of the grape haematochrome every time obtained after purification is 30～35g, therefore the amount of every gram of adsorbable grape haematochrome of alginic acid is in 154～180mg scope, if directly adsorbed with alginic acid powder, so alginic acid absorbability only has 44～56mg/g, so, material provided by the invention has a clear superiority on absorbability, this is mainly attributed to alginic acid and presents the state of high degree of dispersion in compound adsorbing material.
Accompanying drawing explanation
The SEM image of Fig. 1 melamine sponge/compound adsorbing material of alginic acid.
Claims (5)
1. melamine sponge/compound adsorbing material of alginic acid, it is characterized in that this material had both had the through duct of three-dimensional net structure and 100 μm, having again the through shape thin film of alginic acid multilamellar of about 1 μ m-thick, two kinds of patterns intert mutually, constitute stable macroporous structure.
2. melamine sponge according to claim 1/compound adsorbing material of alginic acid, it is characterised in that the specific surface area of described polymer reaches 52.6～61.4m2/ g, alginic acid content is in 52～58wt.% scope.
3. melamine sponge according to claim 1 and 2/compound adsorbing material of alginic acid, it is characterised in that described material can rapidly and efficiently separate grape haematochrome by globality adsorption column submode.
4. the compound adsorbing material preparation method of melamine sponge/alginic acid described in a claim 1, it is characterised in that step is followed successively by:
(1) melamine sponge is immersed in sodium alginate aqueous solution 1～2 hour；
(2) put into rapidly after taking out in the sulfuric acid solution of pH=3～4 and soak 2～3 hours, place in the clear water under room temperature and rinse 4～5 hours；
(3) being placed under room temperature by complex ventilation natural drying, after 3～4 days, complex forms macroporous structure as shown in Figure 1.
5. preparation method according to claim 4, it is characterised in that the viscosity of sodium alginate used itself is 200 ± 20mpa.s, the concentration of institute's water distribution solution is 3～4wt.% scope.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106139816A (en) * | 2016-07-21 | 2016-11-23 | 中国科学院海洋研究所 | A kind of application of low viscosity algin |
| CN108774337A (en) * | 2018-06-22 | 2018-11-09 | 南京林业大学 | A kind of hydrophobically modified method of melamine sponge and products thereof and application |
| US20210268447A1 (en) * | 2016-03-03 | 2021-09-02 | Versitech Limited | Gravity-driven chitosan-enhanced melamine sponge for stable ultrafast filtration |
| CN115888669A (en) * | 2022-11-24 | 2023-04-04 | 南京信息工程大学 | Functionalized sponge-based wastewater phosphorus removal adsorbent and preparation method thereof |
| CN116618030A (en) * | 2023-06-07 | 2023-08-22 | 华东理工大学 | Preparation method of melamine sponge modified adsorbent and application of melamine sponge modified adsorbent in cationic dye wastewater treatment |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20210268447A1 (en) * | 2016-03-03 | 2021-09-02 | Versitech Limited | Gravity-driven chitosan-enhanced melamine sponge for stable ultrafast filtration |
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| CN108774337A (en) * | 2018-06-22 | 2018-11-09 | 南京林业大学 | A kind of hydrophobically modified method of melamine sponge and products thereof and application |
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| CN115888669A (en) * | 2022-11-24 | 2023-04-04 | 南京信息工程大学 | Functionalized sponge-based wastewater phosphorus removal adsorbent and preparation method thereof |
| CN116618030A (en) * | 2023-06-07 | 2023-08-22 | 华东理工大学 | Preparation method of melamine sponge modified adsorbent and application of melamine sponge modified adsorbent in cationic dye wastewater treatment |
| CN116618030B (en) * | 2023-06-07 | 2024-06-18 | 华东理工大学 | Preparation method of melamine sponge modified adsorbent and application of melamine sponge modified adsorbent in cationic dye wastewater treatment |
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