CN102728324A - Polysaccharide decoloring composite material - Google Patents
Polysaccharide decoloring composite material Download PDFInfo
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- CN102728324A CN102728324A CN2011100818223A CN201110081822A CN102728324A CN 102728324 A CN102728324 A CN 102728324A CN 2011100818223 A CN2011100818223 A CN 2011100818223A CN 201110081822 A CN201110081822 A CN 201110081822A CN 102728324 A CN102728324 A CN 102728324A
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Abstract
The invention relates to a composite material for decoloring treatment during the polysaccharide refining process. A preparation method of the composite material comprises the following steps of: washing, drying, crushing, mixing a sieved peanut shell powder with a phosphoric acid solution, adding an aqueous solution of an aluminium-containing compound, stirring and kneading, carrying out extrusion moulding on moulding equipment, putting into a drying box for drying, putting into an electric resistance furnace to carry out heat treatment without air so as to obtain a granular material, dissolving silver nitrate and glucose in water, continuously stirring, adding the above granular material therein, continuously stirring and mixing, removing a filtrate, putting into the drying box for drying, and carrying out heating reduction to prepare the polysaccharide decolouring composite material. By the utilization of the material for decoloring a colored polysaccharide aqueous solution of plants such as ginseng, matrimony vine, pumpkin, mushroom, Mythic Fungus and the like, the decoloring efficiency is high, the loss of polysaccharide is little, and the decoloring material is easy to regenerate.
Description
Technical field
The present invention relates to a kind of composite that the refinishing polyose process is decoloured and handled that is used for, belong to technical field of biochemical industry.
Background technology
Polysaccharide is extremely wide in distributed in nature, and is also very important.Has plenty of the constituent that constitutes the animals and plants skeleton structure, like cellulose; Has plenty of nutrient, like glycogen and starch as the animals and plants storage; What have has a special biologically active, as the heparin in the human body blood coagulation resisting function is arranged, and the polysaccharide in the pneumococcus cell membrane has antigenic action.The structural units of polysaccharide is a monose, and the polysaccharide relative molecular mass necessarily is connected with glycosidic bond between the structural units from several ten thousand to several, can be linked to be straight chain, also can form side chain.
The polysaccharide that has physiological function at present mainly extracts from animals and plants and separates, and is wherein particularly important with the water-soluble polysaccharide that from plant, extracts.Representational plant polyose has panaxan, LBP-X, squash polyoses, tea polysaccharide, lentinan, coriolan, pachymaran, GL-B etc.The natural polysaccharide of purifying is white; Dry, but owing to the source difference of polysaccharide and the defective of method for distilling, add the complexity of plant tissue composition; And special natures such as the big viscosity of polysaccharide molecular weight is bigger; Usually making the polysaccharide liquid that obtains is brown, redness or yellow etc., and this not only extracts to polysaccharide and has caused very big difficulty, and in further it being carried out processes such as separation and purification, qualitative, quantitative analysis and structure determination, very big influence is arranged all.Therefore, decolouring is a vital link in the refinishing polyose process to polysaccharide.
Fat-soluble pigment is mainly the tetraterpenes derivative, and this type pigment is water insoluble, is soluble in ethanol, EC equal solvent; This type polysaccharide can be removed in skimming processes, to plant tissue can be earlier with the benzinum degreasing that refluxes, and then with 95% alcohol reflux degreasing, when removing lipid material, some fat-soluble pigments also are removed.Water colo(u)r such as pattern glucoside, water soluble and ethanol are insoluble to organic solvents such as EC, can be by charcoal absorption, color changes with the difference of pH; This type polysaccharide can be dissolved in the water when hot water lixiviate polysaccharide, and when using the precipitation with alcohol polysaccharide again, pigment is with regard to staying in the supernatant and remove.Yet; Polyphenols, polyphenol oxidase enzyme and and other coloring matter of combining of polysaccharide in above-mentioned separation process, be difficult to remove, be the coloring matter that mainly removes in the refinishing polyose decolorization, domestic and foreign literature is more to the report of refinishing polyose decolouring; But because the difference of vegetable material; Discoloration method also is not quite similar, and at present, removing the comparatively ripe technology of these materials has following three kinds.(1) activated carbon decolorizing: this is the most frequently used discoloration method; It relies on Van der Waals force that pigment is adsorbed onto activated carbon surface, and the particle of active carbon is littler, and its surface area is bigger; Adsorption capacity is stronger, so active carbon is divided into granular activated carbon, Powdered Activated Carbon, super fine activated carbon etc. with granular size.But, for the natural polysaccharide that extractions such as animal, plant obtain, generally speaking, avoid handling with activated carbon decolorizing, because active carbon can adsorb polysaccharide, cause polysaccharide loss.(2) resin decolorization: this is a kind of discoloration method that new development is got up, and its good decolorizing effect is suitable for the system that treating capacity is little, viscosity is little, pigment content is less; Otherwise be prone to cause resin stain; The regeneration difficulty, the resin cost is higher in addition, must screen eluant, eluent with thin-layer chromatography before the experiment; Carry out upper prop, wash-out then, the production cycle is longer.(3) decolour with oxidant: some pigment such as phenols and derivative thereof, in alkaline solution, be in peony, the neutral solution and take on a red color, be orange-yellow in the acid solution, the alkalescence of solution is strong more, and color is dark more; Experiment showed, that when the approaching neutrality of solution the stripping that helps pigment is with stable.This type material contains unsaturated double-bond, light base, aromatic rings etc. more, under alkali condition, can decolour with oxidant reaction.But this method only is suitable for comparatively stable and is difficult for oxidized system decolouring.
Summary of the invention
The deficiency that the objective of the invention is to overcome in the past technology provides a kind of refinishing polyose process composite of handling and preparation method thereof that decolours that is used for.To the processing of decolouring of multiple thick polysaccharide solution, show that decolorizing efficiency height, polysaccharide loss are few, decoloring material characteristics such as regeneration easily with this material.
The preparation method of polysaccharide decolouring composite of the present invention is:
The phosphoric acid solution of peanut hull meal that (1) will clean, dry, pulverize, sieves and mass fraction 30%～85%; It by peanut hull meal and phosphoric acid solution mass ratio 0.8～2.8: 1 mixed; Stir kneading 1～2 hour down at 50～100 ℃; The aqueous solution that adds aluminum contained compound continues to stir and mediated 1～2 hour;
(2) with the extrusion modling on former of above-mentioned compound, and place 80～120 ℃ of dryings of drying box 1.5～2.5 hours, place 360～500 ℃ of resistance furnace secluding airs heat treatment 2～3 hours then, obtain granular materials;
(3) silver nitrate and glucose is soluble in water, under constantly stirring, above-mentioned granular materials is added wherein; Continued to mix 1～2 hour; Discard filtrating and directly place drying box to dry, and under 160～200 ℃, add thermal reduction 5～10 minutes, promptly get polysaccharide decolouring composite.
Wherein, the aluminum contained compound that uses in the step (1) is meant inorganic aluminate or organo-aluminum compound or their mixture.The granular materials of extrusion modling is that maximum particle diameter is no more than 3 millimeters sphere or cylindricality or goose is avette or sheet or bar shaped particle in the step (2).The mass fraction of Ag is 1～6% in the polysaccharide decolouring composite that obtains in the step (3), Al
2O
3Mass fraction be 15～35%.
The specific embodiment
Embodiment 1
The phosphoric acid solution of peanut hull meal that (1) will clean, dry, pulverize, sieves and mass fraction 32%; It by peanut hull meal and phosphoric acid solution mass ratio 0.9: 1 mixed; Stir kneading 1 hour down at 60 ℃, add an amount of aqueous solution of aluminum nitrate, continue to stir and mediated 2 hours;
(2) above-mentioned compound is squeezed into the about 2 millimeters spheric granules of particle diameter on former, and placed 85 ℃ of dryings of drying box 2.5 hours, place 400 ℃ of resistance furnace secluding airs heat treatment 2 hours then, obtain granular materials;
(3) an amount of silver nitrate and glucose is soluble in water, under constantly stirring, above-mentioned granular materials is added wherein; Continued to mix 1 hour; Discard filtrating and directly place drying box to dry, and under 170 ℃, add thermal reduction 6 minutes, promptly get polysaccharide decolouring composite.
Analyze: the gained material is carried out constituent analysis, and the mass fraction that records Ag is 2.5%, Al
2O
3Mass fraction be 25%.
Use: use this polysaccharide decolouring composite to load internal diameter and be 20mm length 200mm glass column, in the time of 43 ℃ to panaxan's processing of decolouring, percent of decolourization 95%, polysaccharide recovery 96%.
Embodiment 2
The phosphoric acid solution of peanut hull meal that (1) will clean, dry, pulverize, sieves and mass fraction 45%; It by peanut hull meal and phosphoric acid solution mass ratio 1: 1 mixed; Stir kneading 1 hour down at 55 ℃, add the aqueous solution of an amount of aluminium chloride, continue to stir and mediated 2 hours;
(2) above-mentioned compound is squeezed into the about 1.8 millimeters spheric granules of particle diameter on former, and placed 85 ℃ of dryings of drying box 1.5 hours, place 380 ℃ of resistance furnace secluding airs heat treatment 3 hours then, obtain granular materials;
(3) an amount of silver nitrate and glucose is soluble in water, under constantly stirring, above-mentioned granular materials is added wherein; Continued to mix 1 hour; Discard filtrating and directly place drying box to dry, and under 165 ℃, add thermal reduction 7 minutes, promptly get polysaccharide decolouring composite.
Analyze: the gained material is carried out constituent analysis, and the mass fraction that records Ag is 3.1%, Al
2O
3Mass fraction be 22%.
Use: this polysaccharide decolouring composite is mixed with polysaccharide solution, and wherein the decolour mass ratio of composite and polysaccharide solution of polysaccharide is 8%, under 45 ℃ to the LBP-X processing of decolouring, percent of decolourization 94%, polysaccharide recovery 97%.
Embodiment 3
The phosphoric acid solution of peanut hull meal that (1) will clean, dry, pulverize, sieves and mass fraction 82%; It by peanut hull meal and phosphoric acid solution mass ratio 2.6: 1 mixed; Stir kneading 1.5 hours down at 65 ℃, add the aqueous solution of an amount of aluminum sulfate, continue to stir and mediated 1 hour;
(2) above-mentioned compound is squeezed into the about 1 millimeter cylindrical particle that is about 2.8 millimeters of radius on former, and placed 115 ℃ of dryings of drying box 1.5 hours, place 480 ℃ of resistance furnace secluding airs heat treatment 2 hours then, obtain granular materials;
(3) an amount of silver nitrate and glucose is soluble in water, under constantly stirring, above-mentioned granular materials is added wherein; Continued to mix 1.5 hours; Discard filtrating and directly place drying box to dry, and under 185 ℃, add thermal reduction 7 minutes, promptly get polysaccharide decolouring composite.
Analyze: the gained material is carried out constituent analysis, and the mass fraction that records Ag is 5%, Al
2O
3Mass fraction be 32%.
Use: this polysaccharide decolouring composite is mixed with polysaccharide solution, and wherein the decolour mass ratio of composite and polysaccharide solution of polysaccharide is 9%, under 45 ℃ to the tea polysaccharide processing of decolouring, percent of decolourization 96%, polysaccharide recovery 97%.
Embodiment 4
The phosphoric acid solution of peanut hull meal that (1) will clean, dry, pulverize, sieves and mass fraction 75%; It by peanut hull meal and phosphoric acid solution mass ratio 1.2: 1 mixed; Stir kneading 1 hour down at 75 ℃, add the ethanol water of an amount of aluminium isopropoxide, continue to stir and mediated 1.5 hours;
(2) above-mentioned compound is squeezed into the about 2.9 millimeters post bar shaped particle of maximum particle diameter on former, and placed 105 ℃ of dryings of drying box 1.5 hours, place 450 ℃ of resistance furnace secluding airs heat treatment 3 hours then, obtain granular materials;
(3) an amount of silver nitrate and glucose is soluble in water, under constantly stirring, above-mentioned granular materials is added wherein; Continued to mix 1 hour; Discard filtrating and directly place drying box to dry, and under 195 ℃, add thermal reduction 6 minutes, promptly get polysaccharide decolouring composite.
Analyze: the gained material is carried out constituent analysis, and the mass fraction that records Ag is 1.5%, Al
2O
3Mass fraction be 18%.
Use: this polysaccharide decolouring composite is mixed with polysaccharide solution, and wherein the decolour mass ratio of composite and polysaccharide solution of polysaccharide is 11%, under 45 ℃ to the lentinan processing of decolouring, percent of decolourization 94%, polysaccharide recovery 92%.
Embodiment 5
The phosphoric acid solution of peanut hull meal that (1) will clean, dry, pulverize, sieves and mass fraction 60%; It by peanut hull meal and phosphoric acid solution mass ratio 1.5: 1 mixed; Stir kneading 1.5 hours down at 85 ℃, add the aqueous solution of an amount of aluminum acetate, continue to stir and mediated 2 hours;
(2) above-mentioned compound is squeezed into the about 2.5 millimeters goose ovoid grain of particle diameter on former, and placed 95 ℃ of dryings of drying box 2 hours, place 480 ℃ of resistance furnace secluding airs heat treatment 2 hours then, obtain granular materials;
(3) an amount of silver nitrate and glucose is soluble in water, under constantly stirring, above-mentioned granular materials is added wherein; Continued to mix 1 hour; Discard filtrating and directly place drying box to dry, and under 162 ℃, add thermal reduction 9 minutes, promptly get polysaccharide decolouring composite.
Analyze: the gained material is carried out constituent analysis, and the mass fraction that records Ag is 4.5%, Al
2O
3Mass fraction be 30%.
Use: this polysaccharide decolouring composite is mixed with polysaccharide solution, and wherein the decolour mass ratio of composite and polysaccharide solution of polysaccharide is 8%, under 45 ℃ to the GL-B processing of decolouring, percent of decolourization 95%, polysaccharide recovery 94%.
Embodiment 6
The phosphoric acid solution of peanut hull meal that (1) will clean, dry, pulverize, sieves and mass fraction 70%; It by peanut hull meal and phosphoric acid solution mass ratio 2: 1 mixed; Stir kneading 1 hour down at 95 ℃, add the aqueous solution of an amount of sodium metaaluminate, continue to stir and mediated 1.5 hours;
(2) above-mentioned compound is squeezed into the about 2.2 millimeters square particle of particle diameter on former, and placed 118 ℃ of dryings of drying box 1 hour, place 490 ℃ of resistance furnace secluding airs heat treatment 2 hours then, obtain granular materials;
(3) an amount of silver nitrate and glucose is soluble in water, under constantly stirring, above-mentioned granular materials is added wherein; Continued to mix 1 hour; Discard filtrating and directly place drying box to dry, and under 198 ℃, add thermal reduction 6 minutes, promptly get polysaccharide decolouring composite.
Analyze: the gained material is carried out constituent analysis, and the mass fraction that records Ag is 5.6%, Al
2O
3Mass fraction be 28%.
Use: this polysaccharide decolouring composite is mixed with polysaccharide solution, and wherein the decolour mass ratio of composite and polysaccharide solution of polysaccharide is 7%, under 45 ℃ to the pachymaran processing of decolouring, percent of decolourization 93%, polysaccharide recovery 95%.
Claims (4)
1. polysaccharide decolouring composite, its preparation method is:
The phosphoric acid solution of peanut hull meal that (1) will clean, dry, pulverize, sieves and mass fraction 30%～85%; It by peanut hull meal and phosphoric acid solution mass ratio 0.8～2.8: 1 mixed; Stir kneading 1～2 hour down at 50～100 ℃; The aqueous solution that adds aluminum contained compound continues to stir and mediated 1～2 hour;
(2) with the extrusion modling on former of above-mentioned compound, and place 80～120 ℃ of dryings of drying box 1.5～2.5 hours, place 360～500 ℃ of resistance furnace secluding airs heat treatment 2～3 hours then, obtain granular materials;
(3) silver nitrate and glucose is soluble in water, under constantly stirring, above-mentioned granular materials is added wherein; Continued to mix 1～2 hour; Discard filtrating and directly place drying box to dry, and under 160～200 ℃, add thermal reduction 5～10 minutes, promptly get polysaccharide decolouring composite.
2. a kind of polysaccharide decolouring composite according to claim 1 is characterized in that described aluminum contained compound is meant inorganic aluminate or organo-aluminum compound or their mixture.
3. a kind of polysaccharide decolouring composite according to claim 1, the granular materials that it is characterized in that described extrusion modling is that maximum particle diameter is no more than 3 millimeters sphere or cylindricality or goose is avette or sheet or bar shaped particle.
4. a kind of polysaccharide decolouring composite according to claim 1 is characterized in that the mass fraction of Ag in the described polysaccharide decolouring composite is 1～6%, Al
2O
3Mass fraction be 15～35%.
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| CN2011100818223A CN102728324A (en) | 2011-04-01 | 2011-04-01 | Polysaccharide decoloring composite material |
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| CN2011100818223A CN102728324A (en) | 2011-04-01 | 2011-04-01 | Polysaccharide decoloring composite material |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107879393A (en) * | 2017-11-29 | 2018-04-06 | 北京联合大学 | A kind of lead ion pollution waters restoration material |
| CN108031446A (en) * | 2017-12-20 | 2018-05-15 | 江苏省农业科学院 | A kind of destainer and preparation method for protecting peanut polysaccharide |
| CN109696421A (en) * | 2019-02-21 | 2019-04-30 | 中山出入境检验检疫局检验检疫技术中心 | The content assaying method of total reducing sugar in cordate houttuynia broken wall particle |
| CN111440251A (en) * | 2020-06-01 | 2020-07-24 | 北京联合大学 | Lentinan purification method |
| CN111533822A (en) * | 2020-06-01 | 2020-08-14 | 北京联合大学 | Extraction and decolorization method of ginseng polysaccharide |
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| CN101269871A (en) * | 2008-04-23 | 2008-09-24 | 南京大学 | Method for processing chrome wastewater |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107879393A (en) * | 2017-11-29 | 2018-04-06 | 北京联合大学 | A kind of lead ion pollution waters restoration material |
| CN108031446A (en) * | 2017-12-20 | 2018-05-15 | 江苏省农业科学院 | A kind of destainer and preparation method for protecting peanut polysaccharide |
| CN108031446B (en) * | 2017-12-20 | 2020-09-11 | 江苏省农业科学院 | Destaining solution for protecting peanut polysaccharide and preparation method thereof |
| CN109696421A (en) * | 2019-02-21 | 2019-04-30 | 中山出入境检验检疫局检验检疫技术中心 | The content assaying method of total reducing sugar in cordate houttuynia broken wall particle |
| CN111440251A (en) * | 2020-06-01 | 2020-07-24 | 北京联合大学 | Lentinan purification method |
| CN111533822A (en) * | 2020-06-01 | 2020-08-14 | 北京联合大学 | Extraction and decolorization method of ginseng polysaccharide |
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Application publication date: 20121017 |