CN101497030A - Environment-friendly oxidation type hydrophobic glucomannan adsorption material and preparation method thereof - Google Patents
Environment-friendly oxidation type hydrophobic glucomannan adsorption material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to an environment friendly oxidation type hydrophobic glucomannan adsorption material and a method for preparing the same, and belongs to the technical field of compositions containing glucomannan materials. The adsorption material comprises the following components in portion by weight: 20 to 100 portions of glucomannan, 50 to 500 portions of 0 to 70 percent glucomannan swelling inhibitor, 5 to 100 portions of alkali, 50 to 500 portions of water, and 1 to 20 portions of oxidizing agent. The preparation method comprises that: the glucomannan is swelled in an alkali mixed solvent of the swelling inhibitor, and subjected to acetyl group removing reaction for 1 to 40 hours at a temperature of between 35 and 90 DEG C; the mixed solution is filtered and washed so as to remove the swelling inhibitor and the excessive alkali, and the obtained product is dried at a temperature of between 50 and 100 DEG C for 8 to 24 hours to obtain the hydrophobic glucomannan; the hydrophobic glucomannan is swelled in water, the pH value is adjusted to be 3 to 12, and then the oxidizing agent is added to hydrophobic glucomannan and reacts for 1 to 24 hours; and the obtained mixed solution is filtered, washed and dried at a temperature of between 50 and 100 DEG C for 8 to 24 hours to obtain the oxidation type hydrophobic glucomannan adsorption material. The material has higher selective adsorption capability on heavy-metal ions and radioactive nuclides, and can be widely applied to the adsorption and separation of the heavy-metal ions and radioactive nuclides generated in mining, mining and metallurgy, chemical industry, electroplating, machinery, nuclear industry, environmental protection and restoration, and the like.
Description
(1) technical field
The present invention relates to a kind of eco-friendly oxidation type hydrophobic glucomannan adsorption material and preparation method thereof, belong to the technical field of compositions that contains the Glucomannan material.
(2) background technology
Heavy metal and radioactive wastewater are mainly derived from mining, ore dressing, smelting, plating, chemical industry, machinery, process hides and nuclear industry, after the waste water that contains heavy metal and radionuclide that these industries produce enters natural water body, not only aquatile is constituted a threat to, and precipitation, absorption and food chain may be passed through and constantly enrichment, destroy ecological environment, and finally jeopardize human beings'health.
Heavy metal and radionuclide have the enrichment accumulation property of biological uptake.The aquatile heavy metal of enrichment and radionuclide concentration in vivo can reach that the hundreds of of concentration shift along food chain step by step to tens thousand of times in the surrounding environment medium, simultaneously in biological internal organ long-term accumulation, presents toxicity after reaching certain limit.Therefore, micro heavy and radionuclide promptly have potential danger.When heavy metal and radionuclide are absorbed by organism, outside existing divided by single ion, also can combine with protein, amino acid, aliphatic acid, shuttle acid and the phosphoric acid in the organism, form acylate, inorganic salts and huge legendary turtle compound.And the toxicity of heavy metal ion and radionuclide and compound thereof all is by playing a role with combining of living organism composition generally, and strong more with the organism combination, then toxicity is strong more.Particularly trace, low-activity nucleic enter the internal radiation hazard that organism causes and more and more are subjected to people's attention.Because heavy metal and radionuclide and compound thereof are difficult for metabolism in vivo, thereby can pass through the food chain enrichment.Need remove or reclaim the Another reason of heavy metal ion and radionuclide from waste water, be because some metal and radionuclide have technology importance or have strategic importance, thereby have higher recycling value.
Both at home and abroad the improvement of heavy metal and radionuclide contamination is still improved inadequately with thorough so far, far can not be stopped the pollution of heavy metal wastewater thereby and radionuclide environment.This is because heavy metal and radionuclide which kind of method heavy metal and radioactive wastewater adopt handle all can not make wherein decompose destruction, can only shift the position of its existence or change its physics and chemical form.For example after chemical precipitation is handled, heavy metal in the waste water and radionuclide change insoluble chemical compound into and precipitate from the ionic condition of dissolving, so change in the mud from water.Therefore,, and ignore recycling and the harmless treatment of handling afterproduct, let alone to run off in environment, will make secondary pollution if only note the processing of waste water itself.Absorption method is to reclaim the most effectual way of micro heavy and radionuclide in the waste water, and has advantages such as wide accommodation, good, the recyclable useful heavy metal of treatment effect and radionuclide and sorbing material be reusable.Existing sorbing material comprises active carbon, mineral matter, inorganic salts, synthetic resin etc.Domestic and international widely used adsorbent is an activated carbon, and is little to the adsorption capacity of heavy metal ion and radionuclide though active carbon can adsorb many chemical substances, generally has only 30～40mg/g, and the regeneration difficulty.The adsorption capacity of ion exchange resin is higher, but only some specific ion is had adsorption capacity, and the regeneration difficulty, the price height.The low price of natural zeolite and clay, but lower to the adsorption capacity of heavy metal ion and radionuclide, be generally less than 10mg/g.And clay mineral material processed heavy metal and radionuclide waste water exist Separation of Solid and Liquid difficulty, adsorbent can not reuse, easily cause secondary pollution etc.For this reason; many researchers are devoted to the research and development of novel absorption material; it is very active in recent years natural biomass to be used for the absorption research of heavy metal ion and radionuclide; natural biomass such as microorganism, shitosan and agricultural solid residue are used for the existing many research reports of absorption of water body heavy metal ion and radionuclide; but the adsorption capacity of these materials is not strong; and none setting shape, in industrial application a lot of defectives are arranged still.
Glucomannan is a kind of from plant konjaku, jerusalem artichoke, any of several broadleaf plants lotus root; the natural macromolecule amylose that extracts in the microbial bacterial; comprise glucose and mannose in its molecule; with β-1; the 4-glycosidic bond connects; simultaneously also have the short-chain branch structure on mannose C-3 position, and also have acetyl group (having an acetyl group on per approximately 19 saccharide residues) on the C-6 position, the size of macromolecule water-solubility has been controlled in the existence of these acetyl group.Multifrequency natures such as Glucomannan possess hydrophilic property, gelation, film forming, antibiotic property, edibility, low heat value and the physiological function that some are special can be widely used in environmental protection, food, medicine, chemical industry and biological field.Sufficient, biodegradable as a kind of renewable natural resources source, have chemical modifiable functional group, and have certain complexing of metal ion ability.As renewable resource, its modification and utilization can be saved the bulk petroleum resource on the one hand, the environmental pollution that a large amount of non-degraded synthesized polymer material discarded objects cause can be alleviated on the other hand, the circulation of biomass can be in natural environment, realized after Glucomannan and material modified the discarding thereof.The hydrophobically modified fixation support that is prepared into of Glucomannan can be made into chromatogram and adsorption stuffing.
Take off the acetyl modification by Glucomannan and form three-dimensional net structure, under the effect of oxidant with Glucomannan on C
6The primary hydroxyl group be oxidized to hydroxy-acid group, obtain oxidation type hydrophobic glucomannan adsorption material and possess good hydrophilicity and mechanical strength and water-fast washing, to adapt to industrial operation; Possess the acid and alkali resistance performance, can be handling heavy metal and radionuclide contamination waste water in the pH scope widely; Possesses loose structure, to increase its adsorption capacity to heavy metal ion and radionuclide; Possess good desorption and regeneration performance, in industrial use, can repeatedly reuse,, realize simultaneously the high efficiente callback of heavy metal ion and radionuclide is utilized again to reduce the cost of wastewater treatment.Oxidation type hydrophobic glucomannan adsorption material preparation technology is easy, and product uses back complete biodegradable, environmentally safe.Can be widely used in mining industry, mining and metallurgy, chemical industry, plating, machinery, nuclear industry and environmental protection adsorbs and separates with radionuclide with the heavy metal ion that reparation etc. is produced.
(3) summary of the invention
1, goal of the invention the purpose of this invention is to provide a kind of eco-friendly oxidation type hydrophobic glucomannan adsorption material and preparation method thereof, is the service that large-scale develops and utilizes of renewable resource Glucomannan.
2, technical scheme technical scheme of the present invention is:
A kind of eco-friendly oxidation type hydrophobic glucomannan adsorption material, the weight portion of its component and each component is: 20～100 parts of Glucomannans, concentration are 50～500 parts of 0～70% Glucomannan swelling inhibitor, 5～100 parts in alkali, 50～500 parts in water, 1～20 part in oxidant.
The method of a kind of production environment close friend's oxidation type hydrophobic glucomannan adsorption material in turn includes the following steps: Glucomannan is swollen in the alkaline mixed solvent of swelling inhibitor, 35～90 ℃ of temperature controls carry out deacetylation reaction 1～40 hour; Filter, flush away swelling inhibitor and excessive alkali, 50～100 ℃ of dryings of temperature 8～24 hours, obtain hydrophobic Glucomannan; Hydrophobic Glucomannan is swollen in the water, transfer pH, add oxidant, reacted 1～24 hour in 3～12; Filter to clean,, promptly obtain oxidation type hydrophobic glucomannan adsorption material 50～100 ℃ of dryings of temperature 8～24 hours.
Glucomannan is from plant konjaku, jerusalem artichoke, any of several broadleaf plants lotus root, the Glucomannan that extracts in the microbial bacterial, and average grain diameter is 1～100um.
Described concentration is that 0～70% Glucomannan swelling inhibitor is one or more any combination in methyl alcohol, ethanol, glycerine, butanols, acetone, butanone, the chloroform, is mixed with 0～70% solution with volume ratio.
Described concentration is that 0～70% Glucomannan swelling inhibitor is sodium chloride, ammonium chloride, sodium chloride, sodium sulphate, ferric sulfate, ferrous sulfate, sodium sulfite, sodium acetate, Peracetic acid sodium, natrium citricum, sodium tetraborate, dipotassium tetraborate, with one or more any combination in other sodium salt, the sylvite, be mixed with 0～70% solution with weight ratio.
Alkali is selected one or more any combination in NaOH, potassium hydroxide, calcium hydroxide, calcium oxide, sodium carbonate, potash, sodium acid carbonate, ethylenediamine, quinine and other organic amine, the organic base for use.
Oxidant is selected potassium permanganate for use, potassium peroxydisulfate, sodium peroxydisulfate, ammonium persulfate and other persulfate, any combination of one or more in hydrogen peroxide, benzoyl peroxide, lauroyl peroxide and other peroxide.
By weight ratio with 20～100 parts of Glucomannans, swell in 50～500 parts of 0～70% the Glucomannan swelling inhibitor mixed solutions that are dissolved with 5～100 parts of alkali, 35～90 ℃ of temperature controls carried out deacetylation and cross-linking reaction 1～40 hour; Filter, flush away swelling inhibitor and excessive alkali, 50～100 ℃ of dryings of temperature 8～24 hours, obtain hydrophobic Glucomannan; 20～100 parts of hydrophobic Glucomannans are swollen in 50～500 parts of water, transfer pH, add 1～20 part of oxidant, reacted 1～24 hour in 1～14, under the effect of oxidant with Glucomannan on C
6The primary hydroxyl group be oxidized to hydroxy-acid group; Filter to clean,, promptly obtain oxidation type hydrophobic glucomannan adsorption material 50～100 ℃ of dryings of temperature 8～24 hours.
3, multifrequency nature such as beneficial effect Glucomannan possess hydrophilic property, gelation, film forming, antibiotic property, edibility, low heat value and physiological function that some are special can be widely used in environmental protection, food, medicine, chemical industry and biological field.Sufficient, biodegradable as a kind of renewable natural resources source, have chemical modifiable functional group, and have certain complexing of metal ion ability.As renewable resource, its modification and utilization can be saved the bulk petroleum resource on the one hand, the environmental pollution that a large amount of non-degraded synthesized polymer material discarded objects cause can be alleviated on the other hand, the circulation of biomass can be in natural environment, realized after Glucomannan and material modified the discarding thereof.The raw material sources of oxidation type hydrophobic glucomannan adsorption material preparation are extensive, and cost is low and technology is easy, and absorption-desorption uses back biodegradable, environmentally safe.Need not during preparation to add that any crosslinking agent and grafting agent can synthesize that expansion rate is low, intensity is good is water insoluble, contain the oxidized form glucomannan adsorbing material that enriches carboxyl.
Take off the acetyl modification by Glucomannan and form " tie knot " three-dimensional net structure, thereby eliminated the problem of water-soluble height of Glucomannan and intensity difference, obtain oxidation type hydrophobic glucomannan adsorption material and possess good hydrophilicity and mechanical strength and water-fast washing, can adapt to the industrialization operation.Possess loose structure, can increase its to the adsorption capacity of heavy metal ion and radionuclide can be in pH scope widely to the adsorption treatment of carrying out of heavy metal and radionuclide contamination waste water.
Glucomannan takes off the acetyl modification and forms three-dimensional net structure, under the effect of oxidant with Glucomannan on C
6The primary hydroxyl group be oxidized to hydroxy-acid group, and have higher specific surface, can carry out chemistry to heavy metal ion and radionuclide and separate with physical absorption, have high selective adsorption capacity.Adsorption rate to contents of many kinds of heavy metal ion and radionuclide can reach 80%～99%, less than 1 o'clock desorb can take place in the pH value, and desorption efficiency reaches more than 85%～99%.
The synthetic oxidation type hydrophobic glucomannan adsorption material of this method has kept the granular of original Glucomannan, has very high specific surface; The synthetic hydrophobic glucomannan of this method at utmost is oxidized to carboxylic group with the primary hydroxyl group on the C6 of Glucomannan under the effect of oxidant, the functional group of abundant strong coordination ability is provided for Adsorption of Heavy Metal Ions and radionuclide.
(4) specific embodiment
The present invention realizes that by following concrete implementing measure wherein said raw material umber is parts by weight except that specified otherwise.Below in conjunction with embodiment the present invention is described in further details.
Embodiment 1: by weight ratio with 20 parts of Glucomannans, swell in 50 parts of the 50% methyl alcohol Glucomannan swelling inhibitor mixed solutions that are dissolved with 5 parts of NaOH, 35 ℃ of temperature controls carried out deacetylation and cross-linking reaction 40 hours; Filter, flush away swelling inhibitor and excessive alkali, 50 ℃ of dryings of temperature 24 hours, obtain hydrophobic Glucomannan; 20 parts of hydrophobic Glucomannans are swollen in 50 parts of water, transfer pH, add 1 part of potassium permanganate, reacted 24 hours in 3; Filter to clean,, promptly obtain oxidation type hydrophobic glucomannan adsorption material 50 ℃ of dryings of temperature 24 hours.
Embodiment 2: by weight ratio with 25 parts of Glucomannans, swell in 80 parts of the 60% ethanol Glucomannan swelling inhibitor mixed solutions that are dissolved with 10 parts of potassium hydroxide, 45 ℃ of temperature controls carried out deacetylation and cross-linking reaction 30 hours; Filter, flush away swelling inhibitor and excessive alkali, 60 ℃ of dryings of temperature 20 hours, obtain hydrophobic Glucomannan; 30 parts of hydrophobic Glucomannans are swollen in 70 parts of water, transfer pH, add 2 parts of potassium peroxydisulfates, reacted 18 hours in 4; Filter to clean,, promptly obtain oxidation type hydrophobic glucomannan adsorption material 60 ℃ of dryings of temperature 20 hours.
Embodiment 3: by weight ratio with 30 parts of Glucomannans, swell in 100 parts of the Glucomannan swelling inhibitor mixed solutions of 70% ethanol that is dissolved with 20 parts of NaOH and 10% acetone preparation, 60 ℃ of temperature controls carried out deacetylation and cross-linking reaction 20 hours; Filter, flush away swelling inhibitor and excessive alkali, 70 ℃ of dryings of temperature 17 hours, obtain hydrophobic Glucomannan; 40 parts of hydrophobic Glucomannans are swollen in 00 part of water, transfer pH, add 3 parts of sodium peroxydisulfates, reacted 14 hours in 5; Filter to clean,, promptly obtain oxidation type hydrophobic glucomannan adsorption material 60 ℃ of dryings of temperature 20 hours.
Embodiment 4: by weight ratio with 35 parts of Glucomannans, swell in 150 parts of the 70% acetone Glucomannan swelling inhibitor mixed solutions that are dissolved with 30 parts of calcium oxide, 70 ℃ of temperature controls carried out deacetylation and cross-linking reaction 10 hours; Filter, flush away swelling inhibitor and excessive alkali, 80 ℃ of dryings of temperature 14 hours, obtain hydrophobic Glucomannan; 50 parts of hydrophobic Glucomannans are swollen in 150 parts of water, transfer pH, add 5 parts of ammonium persulfates, reacted 10 hours in 6; Filter to clean,, promptly obtain oxidation type hydrophobic glucomannan adsorption material 60 ℃ of dryings of temperature 20 hours.
Embodiment 5: by weight ratio with 40 parts of Glucomannans, swell in 200 parts of the 70% chloroform Glucomannan swelling inhibitor mixed solutions that are dissolved with 50 parts of calcium hydroxides, 80 ℃ of temperature controls carried out deacetylation and cross-linking reaction 3 hours; Filter, flush away swelling inhibitor and excessive alkali, 90 ℃ of dryings of temperature 10 hours, obtain hydrophobic Glucomannan; 60 parts of hydrophobic Glucomannans are swollen in 200 parts of water, transfer pH, add 5 parts of potassium permanganate and 5 parts of hydrogen peroxide, reacted 5 hours in 7; Filter to clean,, promptly obtain oxidation type hydrophobic glucomannan adsorption material 70 ℃ of dryings of temperature 15 hours.
Embodiment 6: by weight ratio with 50 parts of Glucomannans, swell in 300 parts of the 50% dipotassium tetraborate Glucomannan swelling inhibitor mixed solutions that are dissolved with 60 parts of quinines, 90 ℃ of temperature controls carried out deacetylation and cross-linking reaction 1 hour; Filter, flush away swelling inhibitor and excessive alkali, 100 ℃ of dryings of temperature 8 hours, obtain hydrophobic Glucomannan; 70 parts of hydrophobic Glucomannans are swollen in 250 parts of water, transfer pH, add 10 parts of benzoyl peroxides, reacted 4 hours in 8; Filter to clean,, promptly obtain oxidation type hydrophobic glucomannan adsorption material 80 ℃ of dryings of temperature 14 hours.
Embodiment 7: by weight ratio with 60 parts of Glucomannans, swell in 350 parts of the 40% sodium acetate Glucomannan swelling inhibitor mixed solutions that are dissolved with 70 parts of ethylenediamines, 60 ℃ of temperature controls carried out deacetylation and cross-linking reaction 15 hours; Filter, flush away swelling inhibitor and excessive alkali, 90 ℃ of dryings of temperature 10 hours, obtain hydrophobic Glucomannan; 80 parts of hydrophobic Glucomannans are swollen in 300 parts of water, transfer pH, add 12 parts of lauroyl peroxides, reacted 3 hours in 9; Filter to clean,, promptly obtain oxidation type hydrophobic glucomannan adsorption material 90 ℃ of dryings of temperature 10 hours.
Embodiment 8: by weight ratio with 75 parts of Glucomannans, swell in 300 parts of the Glucomannan swelling inhibitor mixed solutions of 30% sodium sulphate that is dissolved with 80 parts of potash and 5% sodium sulfite preparation, 70 ℃ of temperature controls carried out deacetylation and cross-linking reaction 8 hours; Filter, flush away swelling inhibitor and excessive alkali, 80 ℃ of dryings of temperature 14 hours, obtain hydrophobic Glucomannan; 20～80 parts of hydrophobic Glucomannans are swollen in 350 parts of water, transfer pH, add 10 parts of hydrogen peroxide and 5 parts of benzoyl peroxides, reacted 2 hours in 10; Filter to clean,, promptly obtain oxidation type hydrophobic glucomannan adsorption material 100 ℃ of dryings of temperature 8 hours.
Embodiment 9: by weight ratio with 90 parts of Glucomannans, swell in 500 parts of the aqueous solution that are dissolved with 90 parts of sodium carbonate, 80 ℃ of temperature controls carried out deacetylation and cross-linking reaction 2 hours; Filter, flush away swelling inhibitor and excessive alkali, 100 ℃ of dryings of temperature 8 hours, obtain hydrophobic Glucomannan; 90 parts of hydrophobic Glucomannans are swollen in 400 parts of water, transfer pH, add 10 parts of potassium permanganate and 8 parts of sodium peroxydisulfates, reacted 2 hours in 11; Filter to clean,, promptly obtain oxidation type hydrophobic glucomannan adsorption material 100 ℃ of dryings of temperature 8 hours.
Embodiment 10: by weight ratio with 100 parts of Glucomannans, swell in 500 parts of the Glucomannan swelling inhibitor mixed solutions of 5% sodium chloride that is dissolved with 100 parts of sodium acid carbonates and 10% sodium tetraborate preparation, 90 ℃ of temperature controls carried out deacetylation and cross-linking reaction 1 hour; Filter, flush away swelling inhibitor and excessive alkali, 80 ℃ of dryings of temperature 14 hours, obtain hydrophobic Glucomannan; 100 parts of hydrophobic Glucomannans are swollen in 500 parts of water, transfer pH, add 20 parts of hydrogen peroxide, reacted 1 hour in 12; Filter to clean,, promptly obtain oxidation type hydrophobic glucomannan adsorption material 90 ℃ of dryings of temperature 10 hours.
Claims (7)
1, a kind of eco-friendly oxidation type hydrophobic glucomannan adsorption material is characterized in that, the weight proportion of its each component is: 20～100 parts of Glucomannans, concentration is 50～500 parts of 0～70% Glucomannan swelling inhibitor, 5～100 parts in alkali, 50～500 parts in water, 1～20 part in oxidant.
2, eco-friendly oxidation type hydrophobic glucomannan adsorption material according to claim 1 is characterized in that, described Glucomannan is from plant konjaku, jerusalem artichoke, any of several broadleaf plants lotus root, the Glucomannan that extracts in the microbial bacterial, and average grain diameter is 1～100um.
3, eco-friendly oxidation type hydrophobic glucomannan adsorption material according to claim 1, it is characterized in that, described concentration is that 0～70% Glucomannan swelling inhibitor is one or more any combination in methyl alcohol, ethanol, glycerine, butanols, acetone, butanone, the chloroform, is mixed with 0～70% solution with volume ratio.
4, eco-friendly oxidation type hydrophobic glucomannan adsorption material according to claim 1, it is characterized in that, described concentration is that 0～70% Glucomannan swelling inhibitor is sodium chloride, ammonium chloride, sodium chloride, sodium sulphate, ferric sulfate, ferrous sulfate, sodium sulfite, sodium acetate, Peracetic acid sodium, natrium citricum, sodium tetraborate, dipotassium tetraborate, with one or more any combination in other sodium salt, the sylvite, be mixed with 0～70% solution with weight ratio.
5, eco-friendly oxidation type hydrophobic glucomannan adsorption material according to claim 1, it is characterized in that described alkali is one or more any combination in NaOH, potassium hydroxide, calcium hydroxide, calcium oxide, sodium carbonate, potash, sodium acid carbonate, ethylenediamine, quinine and other organic amine, the organic base.
6, eco-friendly oxidation type hydrophobic glucomannan adsorption material according to claim 1, it is characterized in that, described oxidant is a potassium permanganate, potassium peroxydisulfate, sodium peroxydisulfate, ammonium persulfate and other persulfate, any combination of one or more in hydrogen peroxide, benzoyl peroxide, lauroyl peroxide and other peroxide.
7, the preparation method of the described eco-friendly oxidation type hydrophobic glucomannan adsorption material of a kind of claim 1 the steps include:
The first step with 20～100 parts of Glucomannans, swells in 50～500 parts of 0～70% the Glucomannan swelling inhibitor mixed solutions that are dissolved with 5～100 parts of alkali, and 35～90 ℃ of temperature controls carried out deacetylation and cross-linking reaction 1～40 hour;
Second step, filter, flush away swelling inhibitor and excessive alkali, 50～100 ℃ of dryings of temperature 8～24 hours, obtain hydrophobic Glucomannan;
The 3rd step swelled in 20～100 parts of hydrophobic Glucomannans in 50～500 parts of water, transferred pH in 3～12, added 1～20 part of oxidant, reacted 1～24 hour, under the effect of oxidant with Glucomannan on C
6The primary hydroxyl group be oxidized to hydroxy-acid group;
The 4th step, filter to clean, 50～100 ℃ of dryings of temperature 8～24 hours, promptly obtain oxidation type hydrophobic glucomannan adsorption material.
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