CN105771923B - A kind of melamine sponge/compound sorbing material of alginic acid and preparation method thereof - Google Patents
A kind of melamine sponge/compound sorbing material of alginic acid and preparation method thereof Download PDFInfo
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- CN105771923B CN105771923B CN201410504360.5A CN201410504360A CN105771923B CN 105771923 B CN105771923 B CN 105771923B CN 201410504360 A CN201410504360 A CN 201410504360A CN 105771923 B CN105771923 B CN 105771923B
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Abstract
The present invention is on a kind of melamine sponge and the compound sorbing material of alginic acid and preparation method thereof.Utilize the distinctive three dimensional skeletal structure of commercialization melamine sponge, sodium alginate aqueous solution is introduced into and freezed solidly in acid condition in sponge, again by the method for natural drying by the moisture removal in alginic acid, ultimately form the three-dimensional big pore system of uniqueness, wherein melamine sponge serves mechanically stable and supporting role, and alginic acid is sufficiently disperseed, form multilayer penetration state film, its adsorption efficiency significantly improves, the content of alginic acid is in 52~58wt.% scopes in composite, and specific surface area is in 52.6~61.4m2/ g range, the compound sorbing material can be used as overall adsorption column, for extracting grape red natural coloring matter, obtain preferable effect, be the advantages of this material：Adsorption capacity is strong, easy to operate, and material can be recycled for multiple times, and reduces cost, improves production efficiency.
Description
Technical field
The present invention relates to the polymer adsorbing material field for nature strength, especially a kind of melamine sponge and sea
Compound sorbing material of alginic acid and preparation method thereof, it can be used for rapidly and efficiently extracting grape red natural coloring matter with it.
Background technology
Alginic acid is also known as alginic acid, alginic acid, seaweeds, is a kind of natural polysaccharide being present in brown alga cell membrane.Marine alga
Sour (Alginic acid) is the polysaccharide formed by monose aldehydic acid linear polymerization, and monomer is that β-D- sweet dews aldehydic acid (M) and α-L- are ancient
Sieve uronic acid (G), M and G units are connected with M-M, G-G or M-G combination by Isosorbide-5-Nitrae glycosidic bond turns into block copolymer,
The empirical formula of alginic acid is (C6H8O6)n, molecular weight ranges are from 1 ten thousand to 60 ten thousand.Alginic acid can quickly absorb moisture,
It is used as dehydrating agent and sizing agent in papermaking and textile industry, its main function is being eaten in the form of sodium alginate or sylvite
It is used as emulsifying agent or thickener in product industry and household chemicals industry, in pharmacy industry, alginic acid is conventional auxiliary material, it
Viscosity make it the adhesive of tablet, due to its water-swellable, be used as disintegrant again and tablet be dispersed in human body, or
Being used as dispersant active ingredient turns into suspension into liquid, and alginate is often used as medicinal slow release agent, in dentistry
It is middle to substitute gypsum and rubber with it, tooth mould is made, alginic acid can be used as absorbent to treat heavy metal poisoning in itself.
Melamine sponge is a kind of expanded material formed by melamine and formaldehyde condensation, has more regular three-dimensional bone
Frame structure, also there is higher toughness by modified melamine sponge, simple melamine sponge and alginic acid are difficult as suction
Enclosure material uses, but both, which are cleverly combined together, can but form a kind of brand-new large pore material, and utilizes alginic acid
The characteristic of natural polymer, the extraction available for natural pigment.The present invention provides a kind of melamine sponge and the compound suction of alginic acid
Enclosure material, as shown in figure 1, melamine sponge provides three dimensional skeletal structure, itself has about 100 μm of aperture, can risen its structure
To mechanically stable and supporting role, and alginic acid can then form multilayer penetration state film, and the thickness of film is three-dimensional at 1 μm or so
Skeleton interts mutually with plural layers, forms three-dimensional big pore system.This composite construction not only increases the scattered journey of alginic acid
Degree, so as to improve its adsorption efficiency, while the supporting role that melamine sponge provides makes composite construction permeability good, including making liquid
Portion is easily flowed, thus composite can be used as monolithic devices absorption pillar, and the invention provides application example, it was demonstrated that the material exists
To having extraordinary effect in the extraction of grape haematochrome.
Grape haematochrome is indispensable natural pigment in food industry, and addition is in fruit wine, jam, acidic beverages extensively
In, improve the color and luster of product.
The content of the invention
Primary technical problem to be solved by this invention is to provide a kind of melamine sponge/compound sorbing material of alginic acid,
It can play an important role in the rapidly and efficiently extraction of grape haematochrome.
Another technical problem to be solved by this invention is to provide above-mentioned melamine sponge/compound sorbing material of alginic acid
Preparation method, it is practical, easy to operate, is easy to largely prepare.
Another technical problem to be solved by this invention is to provide a kind of above-mentioned melamine sponge/compound absorption of alginic acid
Concrete application of the material in grape haematochrome extraction.
1st, technical scheme is used by the present invention solves primary technical problem：A kind of melamine sponge/chitosan composite
Sorbing material, its structure have feature as shown in Figure 1, and wherein marine alga acid content both had in 52~58wt.% scopes, the material
There is the insertion duct of three-dimensional net structure and 100 μm, the multilayer penetration state alginic acid film with about 1 μ m-thick, it compares surface
Product reaches 52.6~61.4m2/ g, adsorption efficiency is high, and liquid internally circulates and is easier, and can be easy to wash adsorbent
It is de-, realize being recycled for multiple times for material.
It is beneficial that alginic acid improves the adsorption efficiency of alginic acid, the opposing party with the compound one side of melamine sponge
Face melamine sponge three-dimensional framework serves mechanically stable and supporting role, makes composite construction permeability good, can make liquid quickly
Flowing, thus the composite can be used as globality absorption pillar, operation is significantly improved during nature strength
Efficiency.
2nd, technical scheme is used by the present invention solves another technical problem：A kind of above-mentioned melamine sponge/alginic acid
The preparation method of compound sorbing material, its characterization step are：1) by the sodium alginate of commodity it is soluble in water (viscosity 200 ±
3~4wt.% concentration 20mpa.s) is made into, by commercially available melamine sponge (melamine and foam made of formaldehyde crosslinking reaction
Material, commercialization) it is immersed in sticky solution 1~2 hour；2) sulfuric acid solution of pH=3~4 is put into after taking out rapidly
Middle immersion 2~3 hours, compound is put into clear water and rinsed 4~5 hours under normal temperature；3) compound is placed under normal temperature and led to
Spontaneously dried at wind, inside compounds form macroporous structure as shown in Figure 1 after 3~4 days.
It is beneficial that sodium alginate soln quick solidification in sour environment, is transformed into alginic acid, by normal temperature certainly
Right drying process, multilayer penetration state pattern as shown in Figure 1 can be formed, and film keeps certain in natural drying process
Orientation, together with this pattern and original three-dimensional framework are interspersed, thus alginic acid can not bond it is agglomerating, so as to keep it
Larger specific surface area, its mechanical strength is higher after two kinds of Material claddings, and anti-pressure ability is stronger, and the entirely appropriate monolithic devices that is used for is inhaled
Attached column.
3rd, technical scheme is used by the present invention solves another technical problem：Above-mentioned melamine sponge/alginic acid is compound
Application process of the type sorbing material in the extraction of glucose haematochrome, it is characterised in that some blocks of cylindrical type materials are superimposed upon one
Rise, be placed in a glass columns, form monolithic devices absorption pillar, material solution is infiltrated and flows through the material, extract quilt
It is adsorbed on the skeleton of polymer, then is collected extract by eluting, reaches the purpose of Separation ＆ Purification.
It is beneficial that above-mentioned processing method wants efficient quick than in general direct mixing method, in the absence of diffusion hindered
The problem of, found through overtesting, each gram of alginic acid can adsorb 103~127 milligrams of grape haematochrome, and its adsorption capacity will
The processing method directly mixed with material solution higher than alginic acid.
The advantage of the invention is that：1) new sorbing material aperture is big, is advantageous to liquid flowing, and resistance is small；2) alginic acid
The film that thickness is only 1 μm is formed, good dispersion, specific surface area is big, improves the adsorption efficiency of alginic acid；3) composite construction machine
Tool stability is good, and anti-pressure ability is strong, thus can be adsorbed in a manner of monolithic devices pillar, and operating efficiency is high.
Embodiment
The present invention is described in further detail with reference to embodiments.
It is prepared by sorbing material：
1) sodium alginate of commodity (200 ± 20mpa.s of viscosity) soluble in water is made into 3~4wt.% concentration, by city
The melamine sponge (melamine and foamed material, commercialization made of formaldehyde crosslinking reaction) sold is immersed in sticky solution
In 1~2 hour；
2) compound is put into rapidly in the sulfuric acid solution of pH=3~4 and soaked 2~3 hours, then compound is put into clear water
In rinsed 4~5 hours under normal temperature；
3) compound is placed in into ventilation under normal temperature to spontaneously dry, inside compounds are formed such as Fig. 1 institutes after 3~4 days
The macroporous structure shown, prepared and tested by 6 times, with gravimetric detemination, alginic acid accounts for 52~58wt.% scopes, marine alga in material
The change of acid content comes from the small size change of the variable density and sodium alginate soln concentration of melamine sponge, is surveyed with specific surface instrument
The specific surface area of material is determined in 52.6~61.4m2/ g range.
The extraction of grape haematochrome is carried out by following operating procedure：
A. pre-process, dry red Grape Skin is crushed and crosses 40 mesh sieves；
B. extract, the red Grape Skin of drying of processing is placed in stainless-steel pan by more than, under conditions of stirring, adds 5 times of weights
50% ethanol water is measured, 60 DEG C of stirrings extract 1~2 hour, and filtrate is collected by filtration；Filter residue extracts once by the same method, merges extraction
Take liquid；
C. concentrate, above-mentioned extract is evaporated under reduced pressure and concentrated, reclaim ethanol, obtain pigment solution, and be filtered to remove residue；
D. separate, by above-mentioned pigment solution by made of melamine sponge/compound sorbing material of alginic acid integral post it is (straight
Footpath is 10cm, is highly 100cm, is formed by stacking by 5 pieces of cylindric samples), the volume of pigment solution and the volume of pillar with the ratio between
It should be 1: 1.5~1: 2.0, remaining liquid is finally extruded pillar in 50~60mL/min by flow control with air, outflow
Liquid color substantially shoals, and the color of pillar becomes grape red；
E. elute, with 95% ethanol elution pillar, control same flow velocity, untill efflux does not have color, receive
Collect eluent, be evaporated under reduced pressure, reclaim ethanol, obtain pigment concentrate；
F. dry, will be dried in vacuo under pigment concentrate normal temperature, obtain pigment powder.
Content analysis：
After taking 2.1% citric acid solution 159 to divide (volume) to divide (volume) to mix with 0.16% disodium phosphate soln 41, use
Citric acid solution or disodium phosphate soln are adjusted to pH3.0, and the solution is standby as cushioning liquid, accurately weigh appropriate examination
Sample, so that the absorbance measured is defined between 0.2~0.7,100mL is settled to plus above-mentioned cushioning liquid, in 1cm absorption cells
Determine it and be about the absorbance A at 525nm in maximum absorption wave, blank test, the colourity of sample are used as by the use of above-mentioned cushioning liquid
Value is calculated with equation below
The sample size (g) of colourity=A × 10/
The colourity of grape haematochrome obtained by experiment is not less than FAO/WHO standards
Alkaline colorimetric analysis：
Materials 1g, adds 5% sodium hydroxide solution 100mL, fully shakes up, and takes time solution 30mL, is extracted with 15mL ether,
With spirit of vinegar back extraction ether extraction liquid twice, each 5mL, secondary acetic acid anti-stripping agent is colourless, is illustrated in sample without alkalescence
Pigment.
Material adsorption capacity is assessed：
The dry state density of melamine sponge/compound sorbing material of alginic acid is generally 0.04~0.05g/mL, integral post
Volume is 7.85L, and its quality is 314~393g, average value 353g, is calculated according to the average value 55% of marine alga acid content, sea
The gross weight of alginic acid is 194g, integral post after fully absorption, the grape haematochrome that is obtained every time after eluting, purifying
Measure as 30~35g, therefore the amount of the adsorbable grape haematochrome of every gram of alginic acid is in 154~180mg scopes, if using alginic acid
Powder directly adsorbs, then and alginic acid adsorption capacity only has 44~56mg/g, so, material provided by the invention is in adsorption capacity
On have a clear superiority, this is mainly attributed to the state that high degree of dispersion is presented in alginic acid in compound sorbing material.
Brief description of the drawings
The SEM image of Fig. 1 melamines sponge/compound sorbing material of alginic acid.
Claims (4)
- A kind of 1. melamine sponge/compound sorbing material of alginic acid, it is characterised in that the material both have three-dimensional net structure and 100 μm of insertion duct, there is the multilayer penetration state alginic acid film of 1 μ m-thick again, two kinds of patterns intert mutually, form stabilization Macroporous structure；The specific surface area of described melamine sponge/compound sorbing material of alginic acid reaches 52.6~61.4m2/ g, marine alga acid content In 52~58wt.% scopes.
- 2. the melamine sponge according to claim 1/compound sorbing material of alginic acid, it is characterised in that described melamine sea The compound sorbing material of silk floss/alginic acid can rapidly and efficiently separate grape haematochrome with globality adsorption column submode.
- A kind of 3. preparation method of melamine sponge/compound sorbing material of alginic acid described in claim 1, it is characterised in that step Suddenly it is followed successively by：A) melamine sponge is immersed in sodium alginate aqueous solution 1~2 hour；B) it is put into rapidly in the sulfuric acid solution of pH=3~4 and soaks 2~3 hours after taking out, is rinsed in the clear water placed under normal temperature 4~5 hours；C) compound is placed in into ventilation under normal temperature to spontaneously dry, compound macroporous structure was formed after 3~4 days.
- 4. preparation method according to claim 3, it is characterised in that the viscosity of sodium alginate used in itself be 200 ± 20mPas, the concentration for matching somebody with somebody the aqueous solution are 3~4wt.% scopes.
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| CN105619968A (en) * | 2016-03-03 | 2016-06-01 | 惠州赛力珑新材料有限公司 | Environment-friendly weather-resistant and stain-resistant wallpaper and making method |
| CN106139816B (en) * | 2016-07-21 | 2019-02-01 | 中国科学院海洋研究所 | A kind of application of low viscosity algin |
| CN108774337B (en) * | 2018-06-22 | 2020-11-27 | 南京林业大学 | Hydrophobic modification method of melamine sponge, product and application thereof |
| 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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| US6723539B1 (en) * | 1998-10-06 | 2004-04-20 | Bioprocessing, Ltd. | Absorbent medium containing particles of chopped cellulose or agarose sponge material having functional groups |
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| CN102068714A (en) * | 2011-01-19 | 2011-05-25 | 北京大学 | Collagen sponge and preparation method thereof |
| CN102675904A (en) * | 2011-03-16 | 2012-09-19 | 杨青松 | Grape skin pigment extracting method |
| CN103087453A (en) * | 2013-01-22 | 2013-05-08 | 广州医学院 | Ionic crosslinked PVA (polyvinyl alcohol) mandruka and preparation method and application thereof |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US6723539B1 (en) * | 1998-10-06 | 2004-04-20 | Bioprocessing, Ltd. | Absorbent medium containing particles of chopped cellulose or agarose sponge material having functional groups |
| CN101445636A (en) * | 2009-01-04 | 2009-06-03 | 武汉理工大学 | A sodium alginate and polyvinyl alcohol compound sponges material and preparation method thereof |
| CN102068714A (en) * | 2011-01-19 | 2011-05-25 | 北京大学 | Collagen sponge and preparation method thereof |
| CN102675904A (en) * | 2011-03-16 | 2012-09-19 | 杨青松 | Grape skin pigment extracting method |
| CN103087453A (en) * | 2013-01-22 | 2013-05-08 | 广州医学院 | Ionic crosslinked PVA (polyvinyl alcohol) mandruka and preparation method and application thereof |
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