CN102029144A - Adsorbent for adsorbing heavy metal ions and dye in waste water and preparation method thereof - Google Patents
Adsorbent for adsorbing heavy metal ions and dye in waste water and preparation method thereof Download PDFInfo
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- CN102029144A CN102029144A CN2009102056481A CN200910205648A CN102029144A CN 102029144 A CN102029144 A CN 102029144A CN 2009102056481 A CN2009102056481 A CN 2009102056481A CN 200910205648 A CN200910205648 A CN 200910205648A CN 102029144 A CN102029144 A CN 102029144A
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Abstract
The invention relates to an adsorbent for adsorbing heavy metal ions and dye in waste water, which is particularly suitable for reluctant printing and dying waste water simultaneously containing heavy metal ions and dye. In the invention, by utilizing the special microcellular structure of bamboo charcoal and the excellent adsorption property of chitosan and using sodium alginate as a cross linker, an adsorbent is developed, which takes the bamboo charcoal as the matrix to load the chitosan and can efficiently remove heavy metal ions and dye in the printing and dying waste water. The specific technical scheme comprises the steps of: after the bamboo charcoal is pretreated, mixing the bamboo charcoal with the sodium alginate by the mass ratio of 3:1, and putting and maintaining the mixture in a water bath at the constant temperature of 80-100DEG C for 14 hours to obtain a bamboo charcoal/ sodium alginate mixture; activating for 120-240min at the temperature of 105-110DEG C; mixing carbide and chitosan into paste by the mass ratio of 2:1, and then adding CH3COOH of certain volume into the paste; quickly stirring and drying; washing until pH is 7.0, and then drying in a drying oven at the temperature of 60DEG C; and smashing, and screening to obtain a BC(Bamboo Charcoal )/CTS (Chitosan) composite adsorbent. When the compound is mixed with FeSO4 by the ratio of 1:1, the adsorption effect of sulfur dye can be improved. The adsorbent is mainly used for treating waste water simultaneously containing heavy metal ions and dye.
Description
Technical field
The present invention relates to a kind of adsorbent that adsorbs heavy metal ions in wastewater and dyestuff, especially bigger to proportion metal ion and reluctant dyeing waste water, enter water body and the pollution that causes is adsorbed through various approach, can efficiently remove the heavy metal ion in the dyeing waste water and the adsorbent of dyestuff simultaneously.
Background technology
The improvement of heavy metal and waste water from dyestuff all is the focus that environmental protection industry (epi) is paid close attention to.Heavy metal can not be by biodegradation, and easily enrichment causes water pollution in water, finally is detrimental to health.Simultaneously, China's printing and dyeing industry mostly is small lot batch manufacture, and major part is intermittently operated, and waste water is discontinuity discharging, thereby the water quality and quantity excursion is very big, and waste water component complexity, concentration height, colourity are dark.The method of removing the heavy metal ion in anhydrating is a lot, and traditional processing method is to adopt chemical precipitation method, membrane filtration, ion-exchange, evaporation absorption method, absorption method and electrolysis etc., but all there is certain defective in these methods.Chemical precipitation method greatly, easily produces secondary pollution to the consumption of reagent; Evaporation absorption method energy consumption is too big; Though ion-exchange and active carbon adsorption effect are better, cost is too high.And traditional adsorbent is to the processing of dyeing waste water, have the advantages that investment is little, method is easy, cost is low, be fit to the processing of middle-size and small-size printing and dyeing mill waste water, it mainly is activated carbon, activated carbon only has absorption property preferably to water-soluble dyes such as the dye of positive ion, direct dyes, acid dyes, reactive dye, but can not remove the colloid hydrophobic dye in the water, and regeneration expense height, the application of activated carbon is restricted.Make a general survey of the production development process of domestic and international water treatment agent, development trend by low molecule to macromolecule, single type to compound, single function to multi-functional.
Bamboo charcoal is a focus in the raw material of wood-charcoal material research field in recent years, has flourishing microcosmic duct, mechanical strength is higher, absorption property is good, can be used as adsorbent, deodorant, conditioning agent, soil conditioner, preserving fruit and vegetable utilizing material, health care product, radioresistance and electromagnetic shielding material and industrial semi-conducting material etc., be a kind of novel function environment-friendly materials.But the easy stripping of the salt in the bamboo charcoal ash content can not be as the purification of water quality filter material of fish breeding water and live fish water, and frangible, re-uses shortcomings such as difficulty after the flushing.Shitosan is the positively charged big molecule of natural biological, easily film forming, nontoxic, corrosion-resistant, easily biological-degradable, anti-microbial property are good, can not cause secondary pollution and aboundresources, contain a large amount of hydroxyls and amino, can it be removed from solution by strong bonded such as hydrogen bond, covalent bond or coordinate bond and printing and dyeing organic molecule, tannic acid molecule, metal ions, have good absorption property.The present invention with sodium alginate as crosslinking agent, by the reformation of pore structure and the physical and chemical performance of hole surface chemical modification change bamboo charcoal, and be the matrix loading chitosan with renewable low-cost resource bamboo charcoal, the good adsorptivity of shitosan, easy film forming are combined with porous, the adsorptivity of bamboo charcoal, develop the efficient compound adsorbent of a kind of environment-friendly bamboo charcoal-shitosan (BC/CTS), this adsorbent has overcome active carbon influence that colourity, the adsorptive selectivity of water is big, regenerative process is complicated, the property is crisp, influence shortcomings such as the turbidity of water, difficult recovery.The adsorbent pore volume obviously increases, and specific area is far longer than chitosan particle, has improved its adsorption capacity to heavy metal ion and dyestuff greatly.
Summary of the invention
One of purpose of patent of the present invention provides a kind of adsorbent that adsorbs heavy metal ions in wastewater and dyestuff.Utilizing resourceful bamboo charcoal to be carrier, is material modified with shitosan, adds sodium alginate as crosslinking agent, preparation (BC/CTS) compound adsorbent.
Two of the purpose of patent of the present invention provides a kind of above-mentioned preparation of adsorbent method.
In order to realize one of foregoing invention patent purpose, the technical scheme that patent of the present invention adopted is: with the bamboo charcoal skeleton is carrier, on its surface, is prepared into the BC/CTS composite with chitosan loaded.Shitosan has excellent biological compatibility, avirulence, nonirritant, contains a large amount of primary amino radicals ,-NH on its strand
2Ionization takes place in group under acid condition, become the NH of positively charged
3 +, be natural polycationic compounds, contain a large amount of carboxyls on the sodium alginate strand, be natural polyanionic compound, under acid condition, shitosan and sodium alginate can form the polyelectrolyte composite membrane by positive and negative charge attraction.
In order to realize two of foregoing invention patent purpose, preparation of adsorbent method of the present invention may further comprise the steps:
1, bamboo charcoal is boiled repeatedly cleaning with deionized water, filter, oven dry is down sieved about 105-110 ℃, continues to dry to constant weight, places drier standby;
2, prepare certain density sodium alginate aqueous solution, standing and defoaming.The shitosan that adds bamboo charcoal and certain mass proportioning while stirring, the acetic acid that adds certain volume behind the furnishing pasty state, stir fast, make the even association reaction of bamboo charcoal, shitosan and sodium alginate, mixture is transferred in the different vessel as required, dry in 60 ℃ of baking ovens, washing is flooded to neutrality, continues oven dry in 60 ℃ of baking ovens, pulverizes, sieve, obtain the BC/CTS combination product of different-grain diameter;
3, with the BC/CTS combination product and the FeSO of different-grain diameter
4According to 1: 1 proportioning, make it constitute good flocculate, improve the adsorption effect of sulfur dye.
The specific embodiment
1, the preliminary treatment of bamboo charcoal: bamboo charcoal is boiled repeatedly to remove the residue on dust and bamboo charcoal surface with deionized water, filter, oven dry is down sieved about 105～110 ℃, continues to dry to constant weight, obtains product A;
2, the preparation of bamboo charcoal/sodium alginate mixture: place baking oven to dry to constant weight for 105～110 ℃ product A (60 order).Bamboo charcoal and sodium alginate by mass ratio be mix at 3: 1 after, constant temperature was placed 14 hours in 80～100 ℃ water-bath, obtained bamboo charcoal/sodium alginate mixture B;
3, activation preparation BC/CTS combination product: at N
2Under the atmosphere, mixture B under 105～110 ℃ of temperature, is activated 120～240min.And with the carbide that obtained with and the shitosan of certain mass proportioning, add the CH of certain volume behind the furnishing pasty state
3COOH, stir fast, make activation bamboo charcoal, shitosan association reaction, as required mixture is transferred in the different vessel, dry in 60 ℃ of baking ovens, washing is flooded to neutrality, in 60 ℃ of baking ovens, continue oven dry, pulverize, sieve, obtain the BC/CTS compound adsorbent of different-grain diameter, can Adsorption of Heavy Metal Ions, acid dyes, reactive dye, premetallized dye and a part of direct dyes.
4, the adsorption function of adsorbent is expanded: with the BC/CTS combination product and the FeSO of different-grain diameter
4According to 1: 1 proportioning, make it constitute good flocculate, can improve the hydrophobic dye adsorption effect of (comprise sulphur red brown BBR, vulcanize deep blue 3R, vulcanize red GGF, vulcanize dark brown GD etc.).Vulcanize alkaline reduzate by acidifying after, the pH value is about 4～5, dyestuff is separated out from solution, and the sulfuration raffinate after the acidifying is precipitated, sediment is recyclable hydrophobic dye after filtration.
5, the regeneration of BC/CTS compound adsorbent: adsorbent is eluted to no adsorbate with the slow vibration of 2% NaOH solution and detects, and then washs to neutral with watery hydrochloric acid, distilled water, dries, and reuses.
The beneficial effect of patent of the present invention is: adopt the blend method for coating to prepare the BC/CTS compound adsorbent, preparation process is simple to operate, energy consumption is low, pollution-free. The actual loading effect of shitosan is better in the composite of preparation, when its load capacity arrives 20%, the absorption effect increases significantly, wherein the quality proportioning of shitosan and sodium alginate is 10: 1 o'clock, compound adsorbent is better to the absorption performance of metal ion, acid dyes, effluent quality is good and more stable after treatment, can not generate spawn in water again simultaneously, causes secondary pollution. As compound adsorbent and FeSO4During according to 1: 1 proportioning, can consist of good flocculate, can improve the absorption effect of hydrophobic dye, simultaneously, vulcanize alkaline reduzate by acidifying after, dyestuff can be separated out from solution, sulfuration raffinate after the acidifying is precipitated, sediment is recyclable hydrophobic dye after filtration, has alleviated the pollution of dyestuff waste water, obtains good economic benefit and environmental benefit. The BC/CTS compound adsorbent is regenerated by sig water, and operating process is easy, quick, efficient is high, functional, reuses adsorption rate after three times and still can arrive originally more than 95%, and can not affect the turbidity of water in the processing procedure.
Claims (5)
1. a composite natural polymeric sorbent is characterized in that: contain a large amount of primary amino radicals ,-NH on the chitosan molecule chain
2Ionization takes place in group under acid condition, become the NH of positively charged
3 +, be natural polycationic compounds, contain a large amount of carboxyls on the sodium alginate strand, be natural polyanionic compound, under acid condition, shitosan and sodium alginate can form the polyelectrolyte composite membrane by positive and negative charge attraction.
2. a kind of composite natural polymeric sorbent according to claim 1 is characterized in that: being carrier with the bamboo charcoal, is material modified with shitosan, adds sodium alginate as crosslinking agent, preparation BC/CTS compound adsorbent.
3. a kind of composite natural polymeric sorbent according to claim 1 and 2, its preparation process condition feature is: bamboo charcoal is boiled repeatedly to remove the residue on dust and bamboo charcoal surface with deionized water, filter, oven dry is down sieved about 105～110 ℃, dries to constant weight, after crossing 60 orders, bamboo charcoal and sodium alginate by mass ratio be mix at 3: 1 after, constant temperature was placed 14 hours in 80～100 ℃ water-bath, obtained bamboo charcoal/sodium alginate mixture.At N
2Under the atmosphere, this mixture under 105～110 ℃ of temperature, is activated 120～240min.And be 2: 1 with carbide and the chitosan mass proportioning that is obtained, add the CH of certain volume behind the furnishing pasty state
3COOH stirs fast, makes activation bamboo charcoal, shitosan association reaction, dries in 60 ℃ of baking ovens, and washing is flooded to pH7.0, continues oven dry in 60 ℃ of baking ovens, pulverizes, and sieves, and obtains the BC/CTS compound adsorbent of different-grain diameter.
4. according to claim 1 or 2 or 3 described a kind of composite natural polymeric sorbents, with the BC/CTS combination product and the FeSO of different-grain diameter
4According to 1: 1 proportioning, constitute good flocculate, improve the adsorption effect of hydrophobic dye.Vulcanize alkaline reduzate by acidifying after, the pH value is about 4～5, dyestuff is separated out from solution, the sulfuration raffinate after the acidifying is precipitated recyclable hydrophobic dye.Adsorbent is eluted to no adsorbate with the slow vibration of 2% NaOH solution and detects, and then washs to neutral with watery hydrochloric acid, distilled water, dries, and reuses.
5. according to claim 1 or 2 or 3 or 4 described a kind of composite natural polymeric sorbents, its preparation of adsorbent method may further comprise the steps:
A) preliminary treatment of bamboo charcoal: bamboo charcoal is boiled repeatedly to remove the residue on dust and bamboo charcoal surface with deionized water, filter, oven dry is down sieved about 105～110 ℃, continues to dry to constant weight, obtains product A;
B) preparation of bamboo charcoal/sodium alginate mixture: place baking oven to dry to constant weight for 105～110 ℃ product A (60 order).Bamboo charcoal and sodium alginate by mass ratio be mix at 3: 1 after, constant temperature was placed 14 hours in 80～100 ℃ water-bath, obtained bamboo charcoal/sodium alginate mixture B;
C) activation preparation BC/CTS combination product: at N
2Under the atmosphere, mixture B under 105～110 ℃ of temperature, is activated 120～240min.And be 2: 1 with carbide and the chitosan mass proportioning that is obtained, add the CH of certain volume behind the furnishing pasty state
3COOH, stir fast, make activation bamboo charcoal, shitosan association reaction, mixture is transferred in the different vessel, dry in 60 ℃ of baking ovens, washing is flooded to neutrality, in 60 ℃ of baking ovens, continue oven dry, pulverize, sieve, obtain the BC/CTS compound adsorbent of different-grain diameter, can Adsorption of Heavy Metal Ions and acid dyes etc.Obtain the BC/CTS compound adsorbent of different-grain diameter, can Adsorption of Heavy Metal Ions and acid dyes etc.
D) adsorption function of adsorbent is expanded: with the BC/CTS combination product and the FeSO of different-grain diameter
4According to 1: 1 proportioning, make it constitute good flocculate, can improve the adsorption effect of hydrophobic dye.
E) regeneration of the recovery of dyestuff and adsorbent: vulcanize alkaline reduzate by acidifying after, the pH value is about 4～5, dyestuff is separated out from solution, and the sulfuration raffinate after the acidifying is precipitated, sediment is recyclable hydrophobic dye after filtration.Adsorbent is eluted to no adsorbate with the slow vibration of 2% NaOH solution and detects, and then washs to neutral with watery hydrochloric acid, distilled water, dries, and reuses.
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