CN103613709A - Method for synthesizing special heavy metal absorption ion resin by using potato starch xanthate as raw material - Google Patents

Method for synthesizing special heavy metal absorption ion resin by using potato starch xanthate as raw material Download PDF

Info

Publication number
CN103613709A
CN103613709A CN201310457568.1A CN201310457568A CN103613709A CN 103613709 A CN103613709 A CN 103613709A CN 201310457568 A CN201310457568 A CN 201310457568A CN 103613709 A CN103613709 A CN 103613709A
Authority
CN
China
Prior art keywords
starch xanthate
heavy metal
temperature
yam starch
metal ions
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201310457568.1A
Other languages
Chinese (zh)
Other versions
CN103613709B (en
Inventor
温国华
巴音其木格
王丹
付渊
温雪
李钰
李在芳
刘嘉
谭小晨
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Beijing Zhongke Emi Technology Co ltd
Original Assignee
Inner Mongolia University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Inner Mongolia University filed Critical Inner Mongolia University
Priority to CN201310457568.1A priority Critical patent/CN103613709B/en
Publication of CN103613709A publication Critical patent/CN103613709A/en
Application granted granted Critical
Publication of CN103613709B publication Critical patent/CN103613709B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

The present invention discloses a method for synthesizing a high water absorption resin from potato starch xanthate grafting acrylic acid and a sodium salt thereof. The method is characterized in that a potato starch xanthate solution, acrylic acid and a sodium salt solution thereof, a N,N'-methylenebisacrylamide solution and initiators (a sodium bisulfate solution and a potassium persulfate solution) are mixed, and are subjected to water bath heating under the protection of nitrogen so as to carry out grafting polymerization at a temperature of 30-45 DEG C to prepare the high water absorption resin, wherein the maximum water absorption of the best product in deionized water achieves 2035 g/g. The high water absorption resin preparation method has the following advantages that: the matrix potato starch xanthate does not require gelatinization, the cost of the acrylic acid and the sodium salt thereof is low, the toxicity is low, the temperature of the grafting polymerization reaction induced by the oxidation reduction system is low, the high temperature reaction is not required, the high water absorption resin synthesis process has characteristics of simpleness, easy operation and low cost, the product performance is excellent, and the method is applicable for large-scale production and product promotion.

Description

Take yam starch xanthate as the synthetic resin dedicated method of Adsorption of Heavy Metal Ions of raw material
Technical field
The present invention relates to a kind of resin dedicated preparation method of functional high molecule material-Adsorption of Heavy Metal Ions who can be applicable to process the fields such as heavy metal contamination, environmental improvement, refer in particular to that to take yam starch xanthate, sodium acrylate, acrylamide be the synthetic resin dedicated a kind of simple method for preparing of Adsorption of Heavy Metal Ions of main raw material.
Background technology
Super absorbent resin (Super Absorbent Resin, be called for short SAR) claims again high water absorbency polymer, is lightly crosslinked three-dimensional netted functional high molecule material in develop in recent years a kind of novel, structure.High hydrophilous resin not only can arrive the water of several thousand times by the heavy hundreds of of specific absorption self, and keep moisture, present gel, and itself is also water insoluble, after being dried, gelatinous mass after absorption can recover its water-retaining capacity, its good stability to light, heat, acid and alkali, also has good biodegradability, and this has determined that it has broad application prospects.On High hydrophilous resin molecule, contain a large amount of hydroxyls, carboxyl, sulfonic group etc., these groups have very strong sequestering action to heavy metal ion, so the sequestrant that High hydrophilous resin can be used as metal ion carries out enrichment, separation and reclaims heavy metal; So being applied to process heavy metal contamination, High hydrophilous resin has very large feasibility.
Because heavy metal has enriching and stability, the feature that is difficult to degrade in environment.Therefore with respect to other pollutions, heavy metal contamination has become the great environmental problem that threatens human survival and development, be necessary to design and synthesize the tailored version polymeric adsorbent of novel applicable Adsorption of Heavy Metal Ions, to meet the social demand that current heavy metal water is seriously polluted and the pollution incident of burst water takes place frequently.
Summary of the invention
The invention provides the resin dedicated preparation method of Adsorption of Heavy Metal Ions that a kind of operating procedure is simple, Adsorption of Heavy Metal Ions ability is strong.Its method and step are as follows:
Take the vinylformic acid of certain mass, take the sodium hydroxide identical with the amount of acrylic substance, with the above-mentioned sodium hydroxide of deionized water dissolving of 2 times of sodium hydroxide quality; In the above-mentioned sodium hydroxide solution of the cooling lower use of ice-water bath and vinylformic acid, with 95% washing with alcohol product of vinylformic acid quality 20%, through suction filtration, oven dry, grinding, obtain solid propenoic acid sodium.
In reaction flask, add yam starch xanthate, the sodium acrylate that yam starch xanthate quality is 3.2~10.4 times, the acrylamide that yam starch xanthate quality is 0.8~2.6 times, the deionized water and stirring that yam starch xanthate quality is 20 times is fully mixed it, then in above-mentioned mixed solution, add potassium persulfate solution that yam starch xanthate quality 1.6~5.6% concentration are 10mg/ml as initiator, stirring makes it to mix, pass into nitrogen, slowly heating, temperature of reaction system is progressively raise, when being raised to 30 ℃, temperature stops stirring, when temperature is raised to 60 ℃, take out product, through shredding, dry, pulverize and to obtain Adsorption of Heavy Metal Ions resin dedicated.Best product is to Pb 2+adsorptive capacity be 756.47mg/g, to Cd 2+adsorptive capacity be 422.69mg/g.
Advantage of the present invention: (1) yam starch xanthate is soluble in water is a kind of good heavy metal ions removal agent; (2) polymeric reaction temperature is low, can reduce energy expenditure; (3) product has higher adsorptive capacity to heavy metal ion.
Embodiment
Embodiment 1: take 2.50g yam starch xanthate, 20.83g sodium acrylate and 4.17g acrylamide, above-mentioned raw materials is dissolved in 50ml deionized water, stirring mixes it, in above-mentioned mixed solution, adding 7ml concentration is the potassium persulfate solution of 10mg/ml, pass into nitrogen, start to stir, slowly heating progressively raises temperature of reaction system, when being raised to 30 ℃, temperature stops stirring, make yam starch xanthate and sodium acrylate and acrylamide carry out copolyreaction, when temperature is raised to 60 ℃, take out product, through shredding, dry, pulverize and to obtain Adsorption of Heavy Metal Ions resin dedicated, the prepared Adsorption of Heavy Metal Ions of the present embodiment is resin dedicated to Pb 2+adsorptive capacity be 718.10mg/g.
Embodiment 2: take 2.50g yam starch xanthate, 20.83g sodium acrylate and 4.17g acrylamide, above-mentioned raw materials is dissolved in 50ml deionized water, stirring mixes it, in above-mentioned mixed solution, adding 13ml concentration is the potassium persulfate solution of 10mg/ml, pass into nitrogen, start to stir, slowly heating progressively raises temperature of reaction system, when being raised to 30 ℃, temperature stops stirring, make yam starch xanthate and sodium acrylate and acrylamide carry out copolyreaction, when temperature is raised to 60 ℃, take out product, through shredding, dry, pulverize and to obtain Adsorption of Heavy Metal Ions resin dedicated, the prepared Adsorption of Heavy Metal Ions of the present embodiment is resin dedicated to Pb 2+adsorptive capacity be 735.02mg/g.
Embodiment 3: take 2.50g yam starch xanthate, 24.00g sodium acrylate and 6.00g acrylamide, above-mentioned raw materials is dissolved in 50ml deionized water, stirring mixes it, in above-mentioned mixed solution, adding 6ml concentration is the potassium persulfate solution of 10mg/ml, pass into nitrogen, start to stir, slowly heating progressively raises temperature of reaction system, when being raised to 30 ℃, temperature stops stirring, make yam starch xanthate and sodium acrylate and acrylamide carry out copolyreaction, when temperature is raised to 60 ℃, take out product, through shredding, dry, pulverize and to obtain Adsorption of Heavy Metal Ions resin dedicated, the prepared Adsorption of Heavy Metal Ions of the present embodiment is resin dedicated to Pb 2+adsorptive capacity be 747.79mg/g.
Embodiment 4: take 2.50g yam starch xanthate, 25.00g sodium acrylate and 5.00g acrylamide, above-mentioned raw materials is dissolved in 50ml deionized water, stirring mixes it, in above-mentioned mixed solution, adding 6ml concentration is the potassium persulfate solution of 10mg/ml, pass into nitrogen, start to stir, slowly heating progressively raises temperature of reaction system, when being raised to 30 ℃, temperature stops stirring, make yam starch xanthate and sodium acrylate and acrylamide carry out copolyreaction, when temperature is raised to 60 ℃, take out product, through shredding, dry, pulverize and to obtain Adsorption of Heavy Metal Ions resin dedicated, the prepared Adsorption of Heavy Metal Ions of the present embodiment is resin dedicated to Pb 2+adsorptive capacity be 756.47mg/g.
Embodiment 5: take 2.50g yam starch xanthate, 20.83g sodium acrylate and 4.17g acrylamide, above-mentioned raw materials is dissolved in 50ml deionized water, stirring mixes it, in above-mentioned mixed solution, adding 9ml concentration is the potassium persulfate solution of 10mg/ml, pass into nitrogen, start to stir, slowly heating progressively raises temperature of reaction system, when being raised to 30 ℃, temperature stops stirring, make yam starch xanthate and sodium acrylate and acrylamide carry out copolyreaction, when temperature is raised to 60 ℃, take out product, through shredding, dry, pulverize and to obtain Adsorption of Heavy Metal Ions resin dedicated, the prepared Adsorption of Heavy Metal Ions of the present embodiment is resin dedicated to Cd 2+adsorptive capacity be 368.33mg/g.
Embodiment 6: take 2.50g yam starch xanthate, 20.83g sodium acrylate and 4.17g acrylamide, above-mentioned raw materials is dissolved in 50ml deionized water, stirring mixes it, in above-mentioned mixed solution, adding 12ml concentration is the potassium persulfate solution of 10mg/ml, pass into nitrogen, start to stir, slowly heating progressively raises temperature of reaction system, when being raised to 30 ℃, temperature stops stirring, make yam starch xanthate and sodium acrylate and acrylamide carry out copolyreaction, when temperature is raised to 60 ℃, take out product, through shredding, dry, pulverize and to obtain Adsorption of Heavy Metal Ions resin dedicated, the prepared Adsorption of Heavy Metal Ions of the present embodiment is resin dedicated to Cd 2+adsorptive capacity be 380.12mg/g.
Embodiment 7: take 2.50g yam starch xanthate, 22.00g sodium acrylate and 5.50g acrylamide, above-mentioned raw materials is dissolved in 50ml deionized water, stirring mixes it, in above-mentioned mixed solution, adding 6ml concentration is the potassium persulfate solution of 10mg/ml, pass into nitrogen, start to stir, slowly heating progressively raises temperature of reaction system, when being raised to 30 ℃, temperature stops stirring, make yam starch xanthate and sodium acrylate and acrylamide carry out copolyreaction, when temperature is raised to 60 ℃, take out product, through shredding, dry, pulverize and to obtain Adsorption of Heavy Metal Ions resin dedicated, the prepared Adsorption of Heavy Metal Ions of the present embodiment is resin dedicated to Cd 2+adsorptive capacity be 325.72mg/g.
Embodiment 8: take 2.50g yam starch xanthate, 26.00g sodium acrylate and 6.50g acrylamide, above-mentioned raw materials is dissolved in 50ml deionized water, stirring mixes it, in above-mentioned mixed solution, adding 6ml concentration is the potassium persulfate solution of 10mg/ml, pass into nitrogen, start to stir, slowly heating progressively raises temperature of reaction system, when being raised to 30 ℃, temperature stops stirring, make yam starch xanthate and sodium acrylate and acrylamide carry out copolyreaction, when temperature is raised to 60 ℃, take out product, through shredding, dry, pulverize and to obtain Adsorption of Heavy Metal Ions resin dedicated, the prepared Adsorption of Heavy Metal Ions of the present embodiment is resin dedicated to Cd 2+adsorptive capacity be 310.76mg/g.

Claims (3)

1. take yam starch xanthate as the synthetic resin dedicated method of Adsorption of Heavy Metal Ions of raw material, be characterised in that: the mass ratio of yam starch xanthate, sodium acrylate, acrylamide, deionized water, Potassium Persulphate is: 1:3.2-10.4:0.8-8:20:0.016-0.056; First, in reaction flask, add yam starch xanthate, sodium acrylate, acrylamide, deionized water and stirring that it is fully mixed, then in above-mentioned mixed solution, add potassium persulfate solution as initiator, stir and make it to mix, pass into nitrogen, slowly heating, temperature of reaction system is progressively raise, when temperature is raised to 30 ℃, stop stirring, when temperature is raised to 60 ℃, take out product, through shredding, dry, pulverize and to obtain Adsorption of Heavy Metal Ions resin dedicated.
2. according to claim 1ly take yam starch xanthate as the synthetic resin dedicated method of Adsorption of Heavy Metal Ions of raw material, it is characterized in that the grafting parent adopting is yam starch xanthate, the grafted monomer of employing is sodium acrylate and acrylamide.
3. according to claim 1ly take yam starch xanthate as the synthetic resin dedicated method of Adsorption of Heavy Metal Ions of raw material, potassium persulfate solution is as initiator, and its concentration is 10mg/ml.
CN201310457568.1A 2013-09-30 2013-09-30 With yam starch xanthate for the resin dedicated method of Material synthesis Adsorption of Heavy Metal Ions Active CN103613709B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201310457568.1A CN103613709B (en) 2013-09-30 2013-09-30 With yam starch xanthate for the resin dedicated method of Material synthesis Adsorption of Heavy Metal Ions

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201310457568.1A CN103613709B (en) 2013-09-30 2013-09-30 With yam starch xanthate for the resin dedicated method of Material synthesis Adsorption of Heavy Metal Ions

Publications (2)

Publication Number Publication Date
CN103613709A true CN103613709A (en) 2014-03-05
CN103613709B CN103613709B (en) 2015-09-16

Family

ID=50164436

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201310457568.1A Active CN103613709B (en) 2013-09-30 2013-09-30 With yam starch xanthate for the resin dedicated method of Material synthesis Adsorption of Heavy Metal Ions

Country Status (1)

Country Link
CN (1) CN103613709B (en)

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105968260A (en) * 2016-06-28 2016-09-28 内蒙古大学 Method for synthesizing absorption of Co<2+> resin by taking carboxymethyl potato starch as raw materials
CN105968262A (en) * 2016-06-28 2016-09-28 内蒙古大学 Method for synthesizing Zn2+ adsorbing resin by using carboxymethyl potato starch as raw material
CN105968261A (en) * 2016-06-28 2016-09-28 内蒙古大学 Method for synthesizing Cu2+ adsorbing resin by using carboxymethyl potato starch as raw material
CN106008824A (en) * 2016-06-28 2016-10-12 内蒙古大学 Method for preparing Ca<2+> ion adsorption resin through one-pot oxidation, alkali gelatinization and graft polymerization by taking potato starch as raw material
CN106008825A (en) * 2016-06-28 2016-10-12 内蒙古大学 Method for preparing Cd<2+> ion adsorption resin through one-pot oxidation, alkali gelatinization and graft polymerization by taking potato starch as raw material
CN106008823A (en) * 2016-06-28 2016-10-12 内蒙古大学 Method for preparing Ag<+> ion adsorption resin through one-pot oxidation, alkali gelatinization and graft polymerization by taking potato starch as raw material
CN106008826A (en) * 2016-06-28 2016-10-12 内蒙古大学 Method for preparing Zn<2+> ion adsorption resin through one-pot oxidation, alkali gelatinization and graft polymerization by taking potato starch as raw material
CN107722180A (en) * 2017-10-01 2018-02-23 桂林理工大学 Cross-linking type BA/AA/AM g xanthic acid is esterified the preparation method of cyanoethyl tapioca
CN108503751A (en) * 2018-02-08 2018-09-07 西北民族大学 The preparation and application of the nano-starch composite particulate material of quaternary ammonium polymer modification

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101638461A (en) * 2009-09-14 2010-02-03 内蒙古大学 Method for synthesizing super absorbent resin containing phosphorus and nitrogen by graft copolymerization reaction of potato starch organic phosphate
CN101974129A (en) * 2010-10-09 2011-02-16 内蒙古大学 Process formula for preparing potassium and nitrogen-containing super absorbent resin by using phosphoric ester of potato starch as raw material
CN101985485A (en) * 2010-10-09 2011-03-16 内蒙古大学 Method for preparing plant growth regulator-containing super absorbent resin
CN103087263A (en) * 2013-01-08 2013-05-08 桂林理工大学 Preparation method of crosslinked AM/AA (acrylamide/acrylic acid) grafted xanthic acid esterification tapioca starch
CN103319614A (en) * 2013-07-02 2013-09-25 内蒙古大学 Method for preparing potato starch xanthate applied to preparing high-absorbent resin

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101638461A (en) * 2009-09-14 2010-02-03 内蒙古大学 Method for synthesizing super absorbent resin containing phosphorus and nitrogen by graft copolymerization reaction of potato starch organic phosphate
CN101974129A (en) * 2010-10-09 2011-02-16 内蒙古大学 Process formula for preparing potassium and nitrogen-containing super absorbent resin by using phosphoric ester of potato starch as raw material
CN101985485A (en) * 2010-10-09 2011-03-16 内蒙古大学 Method for preparing plant growth regulator-containing super absorbent resin
CN103087263A (en) * 2013-01-08 2013-05-08 桂林理工大学 Preparation method of crosslinked AM/AA (acrylamide/acrylic acid) grafted xanthic acid esterification tapioca starch
CN103319614A (en) * 2013-07-02 2013-09-25 内蒙古大学 Method for preparing potato starch xanthate applied to preparing high-absorbent resin

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105968260A (en) * 2016-06-28 2016-09-28 内蒙古大学 Method for synthesizing absorption of Co<2+> resin by taking carboxymethyl potato starch as raw materials
CN105968262A (en) * 2016-06-28 2016-09-28 内蒙古大学 Method for synthesizing Zn2+ adsorbing resin by using carboxymethyl potato starch as raw material
CN105968261A (en) * 2016-06-28 2016-09-28 内蒙古大学 Method for synthesizing Cu2+ adsorbing resin by using carboxymethyl potato starch as raw material
CN106008824A (en) * 2016-06-28 2016-10-12 内蒙古大学 Method for preparing Ca<2+> ion adsorption resin through one-pot oxidation, alkali gelatinization and graft polymerization by taking potato starch as raw material
CN106008825A (en) * 2016-06-28 2016-10-12 内蒙古大学 Method for preparing Cd<2+> ion adsorption resin through one-pot oxidation, alkali gelatinization and graft polymerization by taking potato starch as raw material
CN106008823A (en) * 2016-06-28 2016-10-12 内蒙古大学 Method for preparing Ag<+> ion adsorption resin through one-pot oxidation, alkali gelatinization and graft polymerization by taking potato starch as raw material
CN106008826A (en) * 2016-06-28 2016-10-12 内蒙古大学 Method for preparing Zn<2+> ion adsorption resin through one-pot oxidation, alkali gelatinization and graft polymerization by taking potato starch as raw material
CN107722180A (en) * 2017-10-01 2018-02-23 桂林理工大学 Cross-linking type BA/AA/AM g xanthic acid is esterified the preparation method of cyanoethyl tapioca
CN108503751A (en) * 2018-02-08 2018-09-07 西北民族大学 The preparation and application of the nano-starch composite particulate material of quaternary ammonium polymer modification

Also Published As

Publication number Publication date
CN103613709B (en) 2015-09-16

Similar Documents

Publication Publication Date Title
CN103613709B (en) With yam starch xanthate for the resin dedicated method of Material synthesis Adsorption of Heavy Metal Ions
Jiang et al. Adsorption performance of a polysaccharide composite hydrogel based on crosslinked glucan/chitosan for heavy metal ions
Li et al. Synthesis, characterization and swelling behavior of superabsorbent wheat straw graft copolymers
CN103214616B (en) A kind of preparation method of porous-super-absorberesin resin
Zhou et al. ADSORPTION BEHAVIOR OF Cd 2+, Pb 2+, AND Ni 2+ FROM AQUEOUS SOLUTIONS ON CELLULOSE-BASED HYDROGELS.
CN102153693A (en) Salt-tolerant acrylic absorbent resin and method for preparing same
CN102079823A (en) Method for preparing ethylenediamine modified chitosan composite magnetic microspheres and application thereof
CN109912755B (en) Fulvic acid type three-dimensional network composite material and preparation method and application thereof
CN102225985B (en) Preparation method of macroporous sodium carboxymethylcellulose grafted copolymer with rapid swelling absorption property
Wang et al. Adsorption behaviors of benzonic acid by carboxyl methyl konjac glucomannan gel micropheres cross-linked with Fe3+
CN104262521A (en) Preparation method of styrene-divinylbenzene copolymer hydrophobic catalyst support
CN113000037B (en) Composite microsphere adsorbent for treating ammonia nitrogen and heavy metal composite polluted wastewater in rare earth mining area and preparation method and application thereof
CN102585420B (en) Magnetic expansion adsorption composite material and preparation method thereof
Diao et al. Synthesis and adsorption properties of superabsorbent hydrogel and peanut hull composite
Wen et al. Eco-friendly Enteromorpha polysaccharides-based hydrogels for heavy metal adsorption: From waste to efficient materials
CN102172514A (en) Absorbent material for selectively absorbing As&lt;+5&gt; ions and preparation method thereof
CN102504283B (en) Method for preparing lignosulfonate micro gel
CN102863646B (en) Preparation method for rosin-based porous polymer microsphere
CN105237644A (en) Cellulose with low polymerization degree and preparation method thereof
CN108499543A (en) A kind of preparation method for the cellulose base adsorbent for heavy metal that the degree of polymerization is controllable
Peng et al. Droplet photopolymerization as new strategy for the rapid preparation of hydrogel beads for malachite green removal
CN102604134B (en) Cellulose based water-absorbing and oil-absorbing film and preparation method thereof
CN105295059A (en) Immobilized cationized beta-cyclodextrin chloromethylated polystyrene polymer and method for adsorbing and recovering phenols in industrial wastewater
CN107570120A (en) A kind of preparation method of the modified porous magnetic composite microsphere of DMPS
Ali et al. Science and technology roadmap for adsorption of metallic contaminants from aqueous effluents using biopolymers and its’ derivatives

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
TR01 Transfer of patent right

Effective date of registration: 20240618

Address after: 100176 No.7 Yuanying Road, Zhaofeng industrial base, zhaoquanying Town, Shunyi District, Beijing

Patentee after: Beijing Zhongke Emi Technology Co.,Ltd.

Country or region after: China

Address before: 010021 No. 235 West University Road, Saihan District, Hohhot City, Inner Mongolia Autonomous Region

Patentee before: INNER MONGOLIA University

Country or region before: China