CN106008831A - Method for synthesizing Ag+ adsorption resin from carboxymethyl potato starch and acrylamide - Google Patents
Method for synthesizing Ag+ adsorption resin from carboxymethyl potato starch and acrylamide Download PDFInfo
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- CN106008831A CN106008831A CN201610479875.3A CN201610479875A CN106008831A CN 106008831 A CN106008831 A CN 106008831A CN 201610479875 A CN201610479875 A CN 201610479875A CN 106008831 A CN106008831 A CN 106008831A
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- acrylamide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/264—Synthetic macromolecular compounds derived from different types of monomers, e.g. linear or branched copolymers, block copolymers, graft copolymers
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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Abstract
The invention discloses a method for synthesizing Ag+ adsorption resin from carboxymethyl potato starch and acrylamide. The method is mainly characterized in that firstly, acrylamide is hydrolyzed by means of sodium hydroxide solution, and then water-bath heating is conducted under the protection of nitrogen, so that graft polymerization of carboxymethyl potato starch and parts of hydrolyzed acrylamide is achieved at 30-60 DEG C to prepare the Ag+ adsorption resin. For the best product, Ag+ adsorption capacity is 37.30 mg/g and removal rate is 83.62% in 1000 ml solution with Ag+ concentration of 10 ppm, and Ag+ adsorption capacity is 1563.81 mg/g and removal rate is 97.75% in 1000 ml solution with Ag+ concentration of 400 ppm. The method has the advantages that the parent carboxymethyl potato starch can be dissolved in water so that gelatinization is not needed, the process is simple and easy to implement, graft polymerization reaction temperature is low, practicality is high, and the Ag+ adsorption capacity and removal rate of the prepared Ag+ adsorption resin are high.
Description
Technical field
The present invention relates to a kind of functional high molecule material for field of environmental improvement and adsorb Ag+The preparation method of ion exchange resin, particularly relates to carboxymethyl potato starch, prepares absorption Ag with the acrylamide of sodium hydroxide partial hydrolysis for primary raw material+The method of ion exchange resin.
Background technology
Owing to heavy metal has enriching and stability, being difficult to the feature degraded in the environment, therefore pollute relative to other, heavy metal pollution has become as the great environmental problem threatening human development.Silver simple substance and a small amount of Ag+Ion itself is to human non-toxic, but will produce argyrism after human body excess intake.Ag in waste water+Migration in the environment, diffusion etc. all will pollute natural water, thus to human body and hydrobiological healthy produce serious harm.In commercial production discharge containing Ag+Waste water energy make the mankind touched carcinogenic, the plant of surrounding also can be made to morph, serious harm biology healthy growth.Silver ion has bioconcentration, if containing Ag in a large number+Waste water directly discharge without process if, Ag+Ion then can be enriched with step by step by food chain thus seriously jeopardize the health of people and other biological.Therefore, the effective removal Ag from industrial wastewater of a kind of energy is selected+The method of ion is particularly important.
Summary of the invention
The invention provides that a kind of operating procedure is simple, absorption Ag+Naval stores that ability is strong, adsorbance is high and preparation method thereof.
Its method and step are as follows:
Carboxymethyl potato starch is mixed with a certain amount of deionized water；Weighing a certain amount of acrylamide, it is reacted with acrylamide solution by preparation sodium hydroxide solution by certain degree of hydrolysis；Above-mentioned carboxymethyl potato starch is mixed homogeneously with the acrylamide solution of sodium hydroxide partial hydrolysis with the mixed liquor of deionized water in reaction bulb, add a certain amount of initiator potassium persulfate solution and a certain amount of cross-linking agent N, N ＇-methylene-bisacrylamide solution, stirring is allowed to uniform, it is passed through nitrogen, it is slowly heated, temperature of reaction system is made to be stepped up, polyreaction occurs between 30-60 DEG C, temperature continues rising and reaches insulation 1.5h when 80 DEG C, then take out product, drying, pulverize and i.e. obtain absorption Ag+Resin.The concentration that the initiator potassium persulfate of above-mentioned use is formulated as is the solution of 10mg/ml, cross-linking agent N, and N ＇-methylene-bisacrylamide is formulated as the solution that concentration is 2.5mg/ml.
Product under optimum condition is at 1000mlAg+Concentration be 10ppm solution in Ag+Adsorbance be 37.30mg/g, clearance is 83.62%, at 1000mlAg+Concentration be 400ppm solution in Ag+Adsorbance be 1563.81mg/g, clearance is 97.75%.
Advantages of the present invention:
(1) carboxymethyl potato starch is soluble in water, at absorption Ag+Need not traditional starch gelatinization technique during resin-made is standby, technological process is simple；
(2) polymeric reaction temperature is low, can reduce energy expenditure, practical；
(3) product is to Ag+Advantages of good adsorption effect.
Accompanying drawing explanation
Fig. 1 is carboxymethyl potato starch and acrylamide synthesis absorption Ag+The process chart of resin
Fig. 2 be initiator amount be the Ag of 10ppm to initial concentration+The influence curve of resin absorption amount
Fig. 3 be dosage of crosslinking agent be the Ag of 10ppm to initial concentration+The influence curve of resin absorption amount
Fig. 4 be acrylamide degree of hydrolysis be the Ag of 10ppm to initial concentration+The influence curve of resin absorption amount
Fig. 5 be dissolve carboxymethyl potato starch water consumption be the Ag of 10ppm to initial concentration+The influence curve of resin absorption amount
Fig. 6 is carboxymethyl potato starch and the proportion of acylamide is the Ag of 10ppm to initial concentration+The influence curve of resin absorption amount
Fig. 7 is Ag+The initial concentration influence curve to adsorbance.
Detailed description of the invention
Embodiment 1: weigh 25g acrylamide, is dissolved in 25ml deionized water, weighs 7.04g sodium hydroxide, is dissolved in 15ml deionized water, is added drop-wise in aforesaid propylene amide solution by this sodium hydroxide solution, and under room temperature, stirring makes acrylamide hydrolyze；Weigh 2.5g carboxymethyl potato starch to mix homogeneously with 30ml deionized water, the hydrolyzed solution of acrylamide is mixed homogeneously with carboxymethyl potato starch mixed liquor, add 6ml concentration be the potassium persulfate solution of 10mg/ml, 6ml concentration be the N of 2.5mg/ml, N ＇-methylene-bisacrylamide solution, it is passed through nitrogen, it is slowly heated and makes temperature of reaction system be stepped up, polyreaction occurs at 35 DEG C, it is incubated 1.5h when temperature rises to 80 DEG C, then taking out product, drying, pulverizing obtain adsorbing Ag+Resin, the absorption Ag obtained by the present embodiment+Resin is at 1000mlAg+Concentration be 10ppm solution in Ag+Adsorbance be 34.45mg/g, clearance is 82.72%.
Embodiment 2: weigh 25g acrylamide, is dissolved in 25ml deionized water, weighs 8.45g sodium hydroxide, is dissolved in 15ml deionized water, is added drop-wise in aforesaid propylene amide solution by this sodium hydroxide solution, and under room temperature, stirring makes acrylamide hydrolyze；Weigh 2.5g carboxymethyl potato starch to mix homogeneously with 30ml deionized water, the hydrolyzed solution of acrylamide is mixed homogeneously with carboxymethyl potato starch mixed liquor, add 5ml concentration be the potassium persulfate solution of 10mg/ml, 6ml concentration be the N of 2.5mg/ml, N ＇-methylene-bisacrylamide solution, it is passed through nitrogen, it is slowly heated and makes temperature of reaction system be stepped up, polyreaction occurs at 39 DEG C, it is incubated 1.5h when temperature rises to 80 DEG C, then taking out product, drying, pulverizing obtain adsorbing Ag+Resin, the absorption Ag obtained by the present embodiment+Resin is at 1000mlAg+Concentration be 10ppm solution in Ag+Adsorbance be 26.27mg/g, clearance 79.48%.
Embodiment 3: weigh 25g acrylamide, is dissolved in 25ml deionized water, weighs 7.04g sodium hydroxide, is dissolved in 15ml deionized water, is added drop-wise in aforesaid propylene amide solution by this sodium hydroxide solution, and under room temperature, stirring makes acrylamide hydrolyze；Weigh 2.5g carboxymethyl potato starch to mix homogeneously with 30ml deionized water, the hydrolyzed solution of acrylamide is mixed homogeneously with carboxymethyl potato starch mixed liquor, add 9ml concentration be the potassium persulfate solution of 10mg/ml, 10ml concentration be the N of 2.5mg/ml, N ＇-methylene-bisacrylamide solution, it is passed through nitrogen, it is slowly heated and makes temperature of reaction system be stepped up, polyreaction occurs at 28 DEG C, it is incubated 1.5h when temperature rises to 80 DEG C, then taking out product, drying, pulverizing obtain adsorbing Ag+Resin, the absorption Ag obtained by the present embodiment+Resin is at 1000mlAg+Concentration be 10ppm solution in Ag+Adsorbance be 27.95mg/g, clearance is 76.52%.
Embodiment 4: weigh 15g acrylamide, is dissolved in 25ml deionized water, weighs 4.23g sodium hydroxide, is dissolved in 15ml deionized water, is added drop-wise in aforesaid propylene amide solution by this sodium hydroxide solution, and under room temperature, stirring makes acrylamide hydrolyze；Weigh 2.5g carboxymethyl potato starch to mix homogeneously with 30ml deionized water, the hydrolyzed solution of acrylamide is mixed homogeneously with carboxymethyl potato starch mixed liquor, add 5ml concentration be the potassium persulfate solution of 10mg/ml, 6ml concentration be the N of 2.5mg/ml, N ＇-methylene-bisacrylamide solution, it is passed through nitrogen, it is slowly heated and makes temperature of reaction system be stepped up, polyreaction occurs at 29 DEG C, it is incubated 1.5h when temperature rises to 80 DEG C, then taking out product, drying, pulverizing obtain adsorbing Ag+Resin, the absorption Ag obtained by the present embodiment+Resin is at 1000mlAg+Concentration be 10ppm solution in Ag+Adsorbance be 37.30mg/g, clearance is 83.62%, at 1000mlAg+Concentration be 400ppm solution in Ag+Adsorbance be 1563.81mg/g, clearance is 97.75%.
Embodiment 5: weigh 25g acrylamide, is dissolved in 25ml deionized water, weighs 7.04g sodium hydroxide, is dissolved in 15ml deionized water, is added drop-wise in aforesaid propylene amide solution by this sodium hydroxide solution, and under room temperature, stirring makes acrylamide hydrolyze；Weigh 2.5g carboxymethyl potato starch to mix homogeneously with 35ml deionized water, the hydrolyzed solution of acrylamide is mixed homogeneously with carboxymethyl potato starch mixed liquor, add 5ml concentration be the potassium persulfate solution of 10mg/ml, 6ml concentration be the N of 2.5mg/ml, N ＇-methylene-bisacrylamide solution, it is passed through nitrogen, it is slowly heated and makes temperature of reaction system be stepped up, polyreaction occurs at 31 DEG C, it is incubated 1.5h when temperature rises to 80 DEG C, then taking out product, drying, pulverizing obtain adsorbing Ag+Resin, the absorption Ag obtained by the present embodiment+Resin is at 1000mlAg+Concentration be 10ppm solution in Ag+Adsorbance be 35.84mg/g, clearance is 82.57%.
Claims (3)
1. the invention provides that a kind of operating procedure is simple, absorption Ag+Ability is strong, adsorbance and the high naval stores of clearance and preparation method thereof, and its method and step are as follows:
Carboxymethyl potato starch is mixed with a certain amount of deionized water；Weighing a certain amount of acrylamide, it is reacted with the acrylamide weighed up by preparation sodium hydroxide solution by certain degree of hydrolysis；Above-mentioned carboxymethyl potato starch is mixed homogeneously with the acrylamide solution of sodium hydroxide partial hydrolysis with the mixed liquor of deionized water in reaction bulb, add a certain amount of initiator potassium persulfate and a certain amount of cross-linking agent N, N ＇-methylene-bisacrylamide, stirring is allowed to uniform, it is passed through nitrogen, it is slowly heated, temperature of reaction system is made to be stepped up, polyreaction occurs between 30-60 DEG C, temperature continues rising and reaches insulation 1.5h when 80 DEG C, then take out product, drying, pulverize and i.e. obtain absorption Ag+Resin；It is the solution of 10mg/ml, cross-linking agent N that the initiator potassium persulfate of above-mentioned use is configured to concentration, and N ＇-methylene-bisacrylamide is configured to the solution that concentration is 2.5mg/ml.
The most above-mentioned be Material synthesis resin with carboxymethyl potato starch and acrylamide the absorption Ag for preparing of method+Resin, the product under optimum condition is at 1000mlAg+Concentration be 10ppm solution in Ag+Adsorbance be 37.30mg/g, clearance is 83.62%, at 1000mlAg+Concentration be 400ppm solution in Ag+Adsorbance be 1563.81mg/g, clearance is 97.75%.
3. under optimum condition as described in claim 1, the product of synthesis refers in particular to experimental program preparation absorption Ag as described in claim 1+Resin, wherein carboxymethyl potato starch: dissolving carboxymethyl potato starch water consumption: acrylamide: the water yield of dissolving acrylamide: sodium hydroxide: the water yield of dissolved hydrogen sodium oxide: potassium peroxydisulfate: dissolve the water yield of potassium peroxydisulfate: N, N ＇-methylene-bisacrylamide: dissolve the water yield=1:12:6:10: 1.69:6: the 0.02:2:0.006:2.4 of N, N ＇-methylene-bisacrylamide.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610479875.3A CN106008831A (en) | 2016-06-28 | 2016-06-28 | Method for synthesizing Ag+ adsorption resin from carboxymethyl potato starch and acrylamide |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610479875.3A CN106008831A (en) | 2016-06-28 | 2016-06-28 | Method for synthesizing Ag+ adsorption resin from carboxymethyl potato starch and acrylamide |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101638458A (en) * | 2009-09-14 | 2010-02-03 | 内蒙古大学 | Method for preparing super absorbent resin by using carboxymethyl potato starch as raw material |
| CN101638460A (en) * | 2009-09-14 | 2010-02-03 | 内蒙古大学 | Method for preparing super absorbent resin by graft copolymerization reaction of carboxymethyl potato starch, acrylamide, acrylic acid and sodium salt thereof |
| CN101638456A (en) * | 2009-09-14 | 2010-02-03 | 内蒙古大学 | Method for preparing super absorbent resin with cross-linked structure by using potato starch as raw material |
| CN102093513A (en) * | 2010-12-20 | 2011-06-15 | 昆明理工大学 | Method for preparing absorbent resin by grafting acrylic acid with potato starch |
-
2016
- 2016-06-28 CN CN201610479875.3A patent/CN106008831A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101638458A (en) * | 2009-09-14 | 2010-02-03 | 内蒙古大学 | Method for preparing super absorbent resin by using carboxymethyl potato starch as raw material |
| CN101638460A (en) * | 2009-09-14 | 2010-02-03 | 内蒙古大学 | Method for preparing super absorbent resin by graft copolymerization reaction of carboxymethyl potato starch, acrylamide, acrylic acid and sodium salt thereof |
| CN101638456A (en) * | 2009-09-14 | 2010-02-03 | 内蒙古大学 | Method for preparing super absorbent resin with cross-linked structure by using potato starch as raw material |
| CN102093513A (en) * | 2010-12-20 | 2011-06-15 | 昆明理工大学 | Method for preparing absorbent resin by grafting acrylic acid with potato starch |
Non-Patent Citations (5)
| Title |
|---|
| GHANSHYAM S. CHAUHAN: "Use of biopolymers and acrylamide-based hydrogels for sorption of Cu2+, Fe2+ and Cr6+ ions from their aqueous solutions", 《DESALINATION》 * |
| 冯玉杰，等: "《环境工程中的功能材料》", 31 August 2003, 化学工业出版社 * |
| 吴季怀，等: "《高吸水保水材料》", 31 May 2005, 化学工业出版社 * |
| 张媛等: "羧甲基淀粉基含钾和氮高吸水树脂吸附Fe3+性能研究", 《功能材料与器件学报》 * |
| 祝志峰主编: "《纺织工程化学》", 30 June 2010, 东华大学出版社 * |
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Application publication date: 20161012 |