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 PDFInfo
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- 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
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- Prior art keywords
- starch xanthate
- heavy metal
- temperature
- yam starch
- metal ions
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- ZOOODBUHSVUZEM-UHFFFAOYSA-N ethoxymethanedithioic acid Chemical compound CCOC(S)=S ZOOODBUHSVUZEM-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 239000012991 xanthate Substances 0.000 title claims abstract description 34
- 229920005989 resin Polymers 0.000 title claims abstract description 31
- 239000011347 resin Substances 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 13
- 229910001385 heavy metal Inorganic materials 0.000 title claims description 37
- 239000002994 raw material Substances 0.000 title claims description 14
- 238000010521 absorption reaction Methods 0.000 title abstract description 8
- 229920001592 potato starch Polymers 0.000 title abstract 4
- 230000002194 synthesizing effect Effects 0.000 title abstract 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000000243 solution Substances 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 239000008367 deionised water Substances 0.000 claims abstract description 13
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 13
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 11
- 239000003999 initiator Substances 0.000 claims abstract description 4
- 229920002472 Starch Polymers 0.000 claims description 30
- 150000002500 ions Chemical class 0.000 claims description 30
- 235000019698 starch Nutrition 0.000 claims description 30
- 239000008107 starch Substances 0.000 claims description 30
- 238000003756 stirring Methods 0.000 claims description 30
- 238000001179 sorption measurement Methods 0.000 claims description 27
- PQUXFUBNSYCQAL-UHFFFAOYSA-N 1-(2,3-difluorophenyl)ethanone Chemical compound CC(=O)C1=CC=CC(F)=C1F PQUXFUBNSYCQAL-UHFFFAOYSA-N 0.000 claims description 21
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 21
- 229940047670 sodium acrylate Drugs 0.000 claims description 21
- 239000011259 mixed solution Substances 0.000 claims description 10
- 229920003002 synthetic resin Polymers 0.000 claims description 5
- 239000000057 synthetic resin Substances 0.000 claims description 5
- 239000004159 Potassium persulphate Substances 0.000 claims 1
- 239000000178 monomer Substances 0.000 claims 1
- 235000019394 potassium persulphate Nutrition 0.000 claims 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 abstract description 7
- 238000002360 preparation method Methods 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 3
- 230000008901 benefit Effects 0.000 abstract description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 abstract 3
- 159000000000 sodium salts Chemical class 0.000 abstract 3
- 238000006116 polymerization reaction Methods 0.000 abstract 2
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 239000011159 matrix material Substances 0.000 abstract 1
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 abstract 1
- 230000033116 oxidation-reduction process Effects 0.000 abstract 1
- 239000012266 salt solution Substances 0.000 abstract 1
- WBHQBSYUUJJSRZ-UHFFFAOYSA-M sodium bisulfate Chemical compound [Na+].OS([O-])(=O)=O WBHQBSYUUJJSRZ-UHFFFAOYSA-M 0.000 abstract 1
- 229910000342 sodium bisulfate Inorganic materials 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 230000001988 toxicity Effects 0.000 abstract 1
- 231100000419 toxicity Toxicity 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 230000000274 adsorptive effect Effects 0.000 description 11
- 238000011109 contamination Methods 0.000 description 3
- 230000002745 absorbent Effects 0.000 description 2
- 239000002250 absorbent Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- USNWAMPROKAEIT-UHFFFAOYSA-N [Na].C(C=C)(=O)O Chemical compound [Na].C(C=C)(=O)O USNWAMPROKAEIT-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000005457 ice water Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000003352 sequestering agent Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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
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.
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Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
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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 |
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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 |
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Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
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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 |
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