CN106008835A - Method for synthesizing Zn2+ adsorption resin from carboxymethyl potato starch and acrylamide - Google Patents
Method for synthesizing Zn2+ adsorption resin from carboxymethyl potato starch and acrylamide Download PDFInfo
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- CN106008835A CN106008835A CN201610480306.0A CN201610480306A CN106008835A CN 106008835 A CN106008835 A CN 106008835A CN 201610480306 A CN201610480306 A CN 201610480306A CN 106008835 A CN106008835 A CN 106008835A
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- acrylamide
- solution
- potato starch
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- carboxymethyl potato
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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
-
- 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
Abstract
The invention discloses a method for synthesizing Zn2+ 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 Zn2+ adsorption resin. For the best product, Zn2+ adsorption capacity is 35.77 mg/g and removal rate is 98.78% in 1000 ml solution with Zn2+ concentration of 10 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 Zn2+ adsorption capacity of the prepared Zn2+ adsorption resin is high.
Description
Technical field
The present invention relates to a kind of functional high molecule material for field of environmental improvement and adsorb Zn2+The preparation method of ion exchange resin, particularly relates to carboxymethyl potato starch, prepares absorption Zn with the acrylamide of sodium hydroxide partial hydrolysis for primary raw material2+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.Zinc is many times greater to toxicity comparison people and the homoiothermic animal of Fish and aquatic animal.Zinc is enriched with in soil, can make also to be enriched with in plant and cause the humans and animals evil of edible this plant.With relatively big on the impact of crops particularly Semen Tritici aestivi containing zinc rural sewage disposal farm, Semen Tritici aestivi can be caused to emerge uneven, tiller is few, and plant is short and small, blade is sallow.The zinc of excess also can make soil lose activity, and number of bacteria reduces, and the microbial action in soil weakens.China specifies that the Zn content of drinking water must not exceed 1.0mg/L, and in industrial wastewater, the maximal emission of zinc and compound thereof is 5.0mg/L, and in workshop air, the maximum permissible concentration of zinc oxide is 5.0mg/L.
Summary of the invention
The invention provides that a kind of operating procedure is simple, absorption Zn2+Ability is strong, adsorbance and the high naval stores of clearance 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 to mix with a certain amount of deionized water, 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 Zn2+Resin.It is the solution of 10mg/ml, cross-linking agent N that the initiator potassium persulfate of above-mentioned use is formulated as concentration, and N '-methylene-bisacrylamide is formulated as the solution that concentration is 2.5mg/ml.
Product under optimum condition is at 1000mlZn2+Concentration be 10ppm solution in Zn2+Adsorbance be 35.77mg/g, clearance is 96.05%.At 1000mlZn2+Concentration be 400ppm solution in Zn2+Adsorbance be 1050.22mg/g, clearance is 94.89%.
Advantages of the present invention:
(1) carboxymethyl potato starch is soluble in water, at absorption Zn2+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 Zn2+Advantages of good adsorption effect.
Accompanying drawing explanation
Fig. 1 is carboxymethyl potato starch and acrylamide synthesis absorption Zn2+The process chart of resin
Fig. 2 be initiator amount be the Zn of 10ppm to initial concentration2+The influence curve of resin absorption amount
Fig. 3 be dosage of crosslinking agent be the Zn of 10ppm to initial concentration2+The influence curve of resin absorption amount
Fig. 4 be acrylamide degree of hydrolysis be the Zn of 10ppm to initial concentration2+The influence curve of resin absorption amount
Fig. 5 be dissolve carboxymethyl potato starch water consumption be the Zn of 10ppm to initial concentration2+The influence curve of resin absorption amount
Fig. 6 is carboxymethyl potato starch and the proportion of acylamide is the Zn of 10ppm to initial concentration2+The influence curve of resin absorption amount
Fig. 7 is Zn2+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 Zn2+Resin, the absorption Zn obtained by the present embodiment2+Resin is at 1000mlZn2+Concentration be 10ppm solution in Zn2+Adsorbance be 35.77mg/g, clearance is 96.05%, at 1000mlZn2+Concentration be 400ppm solution in Zn2+Adsorbance be 1050.22mg/g, clearance is 94.89%.
Embodiment 2: weigh 25g acrylamide, is dissolved in 25ml deionized water, weighs 5.63g 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 Zn2+Resin, the absorption Zn obtained by the present embodiment2+Resin is at 1000mlZn2+Concentration be 10ppm solution in Zn2+Adsorbance be 27.95mg/g, clearance, 94.62%.
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 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 28 DEG C, it is incubated 1.5h when temperature rises to 80 DEG C, then taking out product, drying, pulverizing obtain adsorbing Zn2+Resin, the absorption Zn obtained by the present embodiment2+Resin is at 1000mlZn2+Concentration be 10ppm solution in Zn2+Adsorbance be 15.90mg/g, clearance is 91.26%.
Embodiment 4: weigh 12.5g acrylamide, is dissolved in 25ml deionized water, weighs 3.52g 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 Zn2+Resin, the absorption Zn obtained by the present embodiment2+Resin is at 1000mlZn2+Concentration be 10ppm solution in Zn2+Adsorbance be 30.91mg/g, clearance is 95.32%.
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 65ml 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 Zn2+Resin, the absorption Zn obtained by the present embodiment2+Resin is at 1000mlZn2+Concentration be 10ppm solution in Zn2+Adsorbance be 35.20mg/g, clearance is 96.78%.
Claims (3)
1. the invention provides that a kind of operating procedure is simple, absorption Zn2+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 Zn2+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 according to claim 1 be Material synthesis resin with carboxymethyl potato starch and acrylamide the absorption Zn for preparing of method2+Resin, the product under optimum condition is at 1000mlZn2+Concentration be 10ppm solution in Zn2+Adsorbance be 35.77mg/g, clearance is 96.05%, at 1000mlZn2+Concentration be 400ppm solution in Zn2+Adsorbance be 1050.22mg/g, clearance is 94.89%.
3. under process optimum condition described in claim 2, the product of synthesis refers in particular to experimental program preparation absorption Zn as described in claim 12+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=1:12:10:10: the 2.816:6:0.024:2.4:0.006:2.4 of N, N '-methylene-bisacrylamide.
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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 CN201610480306.0A patent/CN106008835A/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 (4)
Title |
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GHANSHYAM S. CHAUHAN,等: "Use of biopolymers and acrylamide-based hydrogels forsorption of Cu2+, Fe2+ and Cr6+ ions from their aqueous solution", 《DESALINATION》 * |
吴季怀,等: "《高吸水保水材料》", 31 March 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: "《环境工程中的功能材料》", 31 August 2003, 东华大学出版社 * |
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