CN104163888A - Method for preparing super absorbent resin by grafting and copolymerizing potato starch oxidized through hydrogen peroxide - Google Patents
Method for preparing super absorbent resin by grafting and copolymerizing potato starch oxidized through hydrogen peroxide Download PDFInfo
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- CN104163888A CN104163888A CN201410322306.9A CN201410322306A CN104163888A CN 104163888 A CN104163888 A CN 104163888A CN 201410322306 A CN201410322306 A CN 201410322306A CN 104163888 A CN104163888 A CN 104163888A
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Abstract
The invention discloses a method for preparing super absorbent resin by grafting and copolymerizing potato starch oxidized through hydrogen peroxide, which comprises the following steps: cooling under ice water-bath, neutralizing acrylic acid by aqueous alkali, mixing with potato starch oxidized through hydrogen peroxide, acrylamide and deionized water, performing water-bath heating under nitrogen protection, and slowly heating to the temperature of 45-55 DEG C and performing graft copolymerization to prepare the super absorbent resin. The highest water-absorbing capacity of 1g of optimum product can reach 3000g/g in 7000 times of deionized water. The preparation of super absorbent resin has the following advantages that no impurity is introduced, raw materials are easily dissolved, a gelatinization process when starch is used in a traditional method is not required during preparation of the super absorbent resin, synthesis technology is simplified, polymerization temperature is low, product water-absorbing capacity is high, nitrogen content is high, product performance is excellent, and the preparation is suitable for large scale production and product popularization.
Description
Technical field
The preparation method who the present invention relates to a kind of functional high molecule material-High hydrophilous resin for fields such as agricultural gardening, physiological hygiene, daily-use chemical industry, building trade, environmental improvements, refers in particular to a kind of novel simple method for preparing taking hydrogen peroxide oxidation yam starch, vinylformic acid, sodium hydroxide or potassium hydroxide as main raw material synthesizing super absorbent resin.
Background technology
Super absorbent resin is lightly crosslinked three-dimensional netted functional high molecule material in develop in recent years a kind of novel, structure.It can absorb the extremely water of several thousand times of own wt hundred times, to the good stability of light, heat, acid and alkali, also has good biodegradability.The responsiveness that High hydrophilous resin stimulates with its water-absorbent, water-retentivity, to external world and the complex ability to heavy metal ion and be used widely, as agricultural gardening, soil improvement, preserve moisture and fertility, hydrogel substrate, physiological hygiene articles for use, medicine medical treatment, oily water separation, sensitive material, sealing material, nursery stock are protected etc.; Utilize the applied research of the aspect such as water swellability, thickening property, moisture-absorbing/releasing, heavy metal ion adsorbed property, accumulation of heat cold insulation of High hydrophilous resin also progressively launching, as building coating environmental protection, daily cosmetic, foodstuffs industry, medicine manufacture, defense technology etc.
High hydrophilous resin Application Areas is constantly expanded, and market demand is increasing.Super absorbent resin is a family macromolecule ionogen, and in water, the water-retaining capacity of the existence meeting remarkably influenced resin of salts substances, has limited its application to a certain extent.Ensureing that SAP has on good water suction and water retention property basis, improving the receptivity of super absorbent resin to salt-containing liquid (as urine, blood, fertilizer water etc.), will be an important topic in super absorbent resin research work from now on.Theoretical investigation work to water absorbing mechanism of absorbent resin also will further be carried out, and instruct this class functional high molecule material to develop to higher level.
Summary of the invention
The invention provides super absorbent resin fat prod that a kind of operating procedure is simple, water-retaining capacity is strong and preparation method thereof.
Its method and step are as follows:
(1) hydrogen peroxide oxidation yam starch is mixed by the mass ratio of 1:4～6 with deionized water; Take the vinylformic acid of 2～10 times of hydrogen peroxide oxidation yam starch quality, take vinylformic acid quality 0.111-0.333 sodium hydroxide (or taking vinylformic acid quality 0.156-0.467 potassium hydroxide doubly) doubly, with the above-mentioned sodium hydroxide of deionized water dissolving (or potassium hydroxide) of 4～6 times of hydrogen peroxide oxidation yam starch quality; In the ice-water bath above-mentioned sodium hydroxide of cooling lower use (or potassium hydroxide) solution and vinylformic acid; Take vinylformic acid quality 0.5-3 acrylamide doubly.
(2) by the mixed solution of above-mentioned hydrogen peroxide oxidation yam starch and deionized water with mix in reaction vessel with acrylic acid solution and the acrylamide of sodium hydroxide (or potassium hydroxide) part neutralization, without additional initiator, add the N that contains hydrogen peroxide oxidation yam starch quality 0.02～0.18%, N ＇-methylene-bisacrylamide solution makees linking agent, it is even that stirring makes it, pass into nitrogen, slowly heating, temperature of reaction system is progressively raise, reaching 50 DEG C stops stirring, then be progressively warmed up to 90 DEG C, be incubated one hour and take out product, drying, pulverize and obtain High hydrophilous resin.Best product 1g high water absorption in the deionized water of 7000 times reaches 2000g/g.
As mentioned above, in the present invention, be sodium hydroxide, potassium hydroxide with vinylformic acid alkali used.The N of preparation, the concentration of N ＇-methylene-bisacrylamide solution is 2mg/ml.
Advantage of the present invention:
(1), without additional initiator, raw material can self serve as initiator, has simplified synthesis technique, and can not introduce any impurity;
(2) hydrogen peroxide oxidation yam starch is soluble in water, does not need gelatinization at High hydrophilous resin in the process of preparing;
(3) polymeric reaction temperature is low, can reduce energy expenditure;
(4) in this product, contain the necessary nitrogen element of plant-growth, also nitrogen element and potassium element can be contained simultaneously, both can, for soil moisture conservation, soil nutrient composition can be increased again, therefore, there is important using value in fields such as agriculture, woods and gardening.
Brief description of the drawings:
Fig. 1 is monomer vinylformic acid and the impact (use in sodium hydroxide and vinylformic acid, degree of neutralization be 50%, securing unit than be 1:1) of acrylamide total mass on High hydrophilous resin water regain
Fig. 2 is the impact (use in sodium hydroxide and vinylformic acid) of the acrylic acid degree of neutralization of monomer on High hydrophilous resin water regain
Fig. 3 is the impact (use in sodium hydroxide and vinylformic acid, degree of neutralization be 50%) of dosage of crosslinking agent on High hydrophilous resin water regain
Fig. 4 is the impact (use in sodium hydroxide and vinylformic acid, degree of neutralization is 50%) of monomer mass comparison High hydrophilous resin water-intake rate
Fig. 5 is monomer vinylformic acid and the impact (use in potassium hydroxide and vinylformic acid, degree of neutralization be 50%) of acrylamide total mass on High hydrophilous resin water regain
Fig. 6 is the impact (use in potassium hydroxide and vinylformic acid, degree of neutralization be 50%) of the acrylic acid degree of neutralization of monomer on High hydrophilous resin water regain
Fig. 7 is the impact (use in potassium hydroxide and vinylformic acid, degree of neutralization be 50%) of dosage of crosslinking agent on High hydrophilous resin water regain
Fig. 8 is the impact (use in potassium hydroxide and vinylformic acid, degree of neutralization is 50%) of monomer mass comparison High hydrophilous resin water-intake rate
Fig. 9 is the technical process that High hydrophilous resin is prepared in the copolymerization of hydrogen peroxide oxidation potato starch graft
Figure 10 is the infrared spectrogram of embodiment 2 prepared High hydrophilous resins
Figure 11 is the infrared spectrogram of embodiment 7 prepared High hydrophilous resins.
Embodiment
Embodiment 1: weigh 3.33g sodium hydroxide, be dissolved in 25.00ml deionized water, in the above-mentioned sodium hydroxide solution of the cooling lower use of ice-water bath and the vinylformic acid of 15.00g (14.30ml).Take 5.00g hydrogen peroxide oxidation yam starch, 15.00g acrylamide, 10.00mg N, N ＇-methylene-bisacrylamide, measure 50.0ml deionized water, all join in reactor, and pour the vinylformic acid having made and sodium salt solution thereof into reactor, under room temperature, stir 1.0h, it is mixed.Under nitrogen protection, stir, heat, control rate of heating simultaneously, bath temperature is slowly raise, stop stirring when temperature reaches 50 DEG C.After this heat up gradually, when after the water boiling in water-bath, continue heating and make it in this temperature range, react 1-2h, stop logical nitrogen, be cooled to room temperature.Product is taken out, cut into fritter, in 40 DEG C of-60 DEG C of baking ovens, dry, originally execute routine prepared High hydrophilous resin water regain and reach 1400g/g.
Embodiment 2: weigh 5.56g sodium hydroxide, be dissolved in 25.00ml deionized water, in the above-mentioned sodium hydroxide solution of the cooling lower use of ice-water bath and (19.05ml) vinylformic acid of 20.00g.Take 5.00g hydrogen peroxide oxidation yam starch, 10.00g acrylamide, 3.00mg N, N ＇-methylene-bisacrylamide, measure 50.0ml deionized water, all join in reactor, and pour the vinylformic acid having made and sodium salt solution thereof into reactor, under room temperature, stir 1.0h, it is mixed.Under nitrogen protection, stir, heat, control rate of heating simultaneously, bath temperature is slowly raise, stop stirring when temperature reaches 52 DEG C.After this heat up gradually, when after the water boiling in water-bath, continue heating and make it in this temperature range, react 1-2h, stop logical nitrogen, be cooled to room temperature.Product is taken out, cut into fritter, in 40 DEG C of-60 DEG C of baking ovens, dry, originally execute routine prepared High hydrophilous resin water regain and reach 1630g/g.
Embodiment 3: weigh 5.56g sodium hydroxide, be dissolved in 25.00ml deionized water, in the above-mentioned sodium hydroxide solution of the cooling lower use of ice-water bath and (14.30ml) vinylformic acid of 15.00g.Take 5.00g hydrogen peroxide oxidation yam starch, 15.00g acrylamide, 10.00mg N, N ＇-methylene-bisacrylamide, measure 50.0ml deionized water, all join in reactor, and pour the vinylformic acid having made and sodium salt solution thereof into reactor, under room temperature, stir 1.0h, it is mixed.Under the protection of nitrogen, stir, heat, control rate of heating simultaneously, bath temperature is slowly raise, after temperature reaches 50 DEG C, stop stirring.After this heat up gradually, when after the water boiling in water-bath, continue heating and make it in this temperature range, react 1-2h, stop logical nitrogen, be cooled to room temperature.Product is taken out, cut into fritter, in 40 DEG C of-60 DEG C of baking ovens, dry, originally execute routine prepared High hydrophilous resin water regain and reach 1500g/g.
Embodiment 4: weigh 5.00g sodium hydroxide, be dissolved in the deionized water of 25.00ml, in the above-mentioned sodium hydroxide solution of the cooling lower use of ice-water bath and (14.30ml) vinylformic acid of 15.00g.Take 5.00g hydrogen peroxide oxidation yam starch, 15.00g acrylamide, 10.00mg N, N ＇-methylene-bisacrylamide, measure 50.0ml deionized water, all join in reactor, and pour the vinylformic acid having made and sodium salt solution thereof into reactor, under room temperature, stir 1.0h, it is mixed.Under the protection of nitrogen, stir, heat, control rate of heating simultaneously, bath temperature is slowly raise, graft copolymerization is fully carried out, after temperature reaches 53 DEG C, stop stirring.After this heat up gradually, when after the water boiling in water-bath, continue heating and make it in this temperature range, react 1-2h, stop logical nitrogen, be cooled to room temperature.Product is taken out, cut into fritter, in 40 DEG C of-60 DEG C of baking ovens, dry, originally execute routine prepared High hydrophilous resin water regain and reach 1300g/g.
Embodiment 5: weigh 6.22g potassium hydroxide, be dissolved in the deionized water of 25.00ml, in the above-mentioned potassium hydroxide solution of the cooling lower use of ice-water bath and 20.00g (19.05ml) vinylformic acid.Take 5.00g hydrogen peroxide oxidation yam starch, 10.00g acrylamide, 7.00mg N, N ＇-methylene-bisacrylamide, measure 50.0ml deionized water, all join in reactor, and pour the vinylformic acid having made and potassium salt soln thereof into reactor, under room temperature, stir 1.0h, it is mixed.Under the protection of nitrogen, stir, heat, control rate of heating simultaneously, bath temperature is slowly raise, graft copolymerization is fully carried out, after temperature reaches 50 DEG C, stop stirring.After this slowly heat up gradually, when after the water boiling in water-bath, continue heating and make it in this temperature range, react 1-2h, stop logical nitrogen, be cooled to room temperature.Product is taken out, cut into fritter, in 40 DEG C of-60 DEG C of baking ovens, dry, originally execute routine prepared High hydrophilous resin water regain and reach 1900g/g.
Embodiment 6: weigh 5.83g potassium hydroxide, be dissolved in 25.00ml deionized water, in the above-mentioned potassium hydroxide solution of the cooling lower use of ice-water bath and the vinylformic acid of 15.00g (14.30ml).Take 5.00g hydrogen peroxide oxidation yam starch, 15.00g acrylamide, 10.00mg N, N ＇-methylene-bisacrylamide, measure 50.0ml deionized water, all join in reactor, and pour the vinylformic acid having made and potassium salt soln thereof into reactor, under room temperature, stir 1.0h, it is mixed.Under nitrogen protection, stir, heat, control rate of heating simultaneously, bath temperature is slowly raise, stop stirring when temperature reaches 50 DEG C.After this slowly heat up gradually, when after the water boiling in water-bath, continue heating and make it in this temperature range, react 1-2h, stop logical nitrogen, be cooled to room temperature.Product is taken out, cut into fritter, in 40 DEG C of-60 DEG C of baking ovens, dry, originally execute routine prepared High hydrophilous resin water regain and reach 1300g/g.
Embodiment 7: weigh 5.60g potassium hydroxide, be dissolved in 25.00ml deionized water, in the above-mentioned potassium hydroxide solution of the cooling lower use of ice-water bath and (14.30.ml) vinylformic acid of 15.00g.Take 5.00g hydrogen peroxide oxidation yam starch, 15.00g acrylamide, 5.00mg N, N ＇-methylene-bisacrylamide, measure 35.0ml deionized water, all join in reactor, and pour the vinylformic acid having made and potassium salt soln thereof into reactor, under room temperature, stir 1.0h, it is mixed.Under nitrogen protection, stir, heat, control rate of heating simultaneously, bath temperature is slowly raise, after temperature reaches 55 DEG C, stop stirring.After this slowly heat up gradually, when after the water boiling in water-bath, continue heating and make it in this temperature range, react 1-2h, stop logical nitrogen, be cooled to room temperature.Product is taken out, cut into fritter, in 40 DEG C of-60 DEG C of baking ovens, dry, originally execute routine prepared High hydrophilous resin water regain and reach 1450g/g.
Embodiment 8: weigh 4.67g potassium hydroxide, be dissolved in 25.00ml deionized water, in the above-mentioned potassium oxide solution of the cooling lower use of ice-water bath and (14.30ml) vinylformic acid of 15.00g.Take 5.00g hydrogen peroxide oxidation yam starch, 15.00g acrylamide, 7.00mg N, N ＇-methylene-bisacrylamide, measure 35.0ml deionized water, all join in reactor, and pour the vinylformic acid having made and potassium salt soln thereof into reactor, under room temperature, stir 1.0h, it is mixed.Under the protection of nitrogen, stir, heat, control rate of heating simultaneously, bath temperature is slowly raise, graft copolymerization is fully carried out, after temperature reaches 53 DEG C, stop stirring.After this slowly heat up gradually, when after the water boiling in water-bath, continue heating and make it in this temperature range, react 1-2h, stop logical nitrogen, be cooled to room temperature.Product is taken out, cut into fritter, in 40 DEG C of-60 DEG C of baking ovens, dry, originally execute routine prepared High hydrophilous resin water regain and reach 1275g/g.
Embodiment 9: weigh 2.91g potassium hydroxide, be dissolved in 25.00ml deionized water, in the above-mentioned potassium oxide solution of the cooling lower use of ice-water bath and (7.14ml) vinylformic acid of 7.50g.Take 5.00g hydrogen peroxide oxidation yam starch, 7.50g acrylamide, 5.00mg N, N ＇-methylene-bisacrylamide, measure 35.0ml deionized water, all join in reactor, and pour the vinylformic acid having made and potassium salt soln thereof into reactor, under room temperature, stir 1.0h, it is mixed.Under the protection of nitrogen, stir, heat, control rate of heating simultaneously, bath temperature is slowly raise, graft copolymerization is fully carried out, after temperature reaches 55 DEG C, stop stirring.After this slowly heat up gradually, when after the water boiling in water-bath, continue heating and make it in this temperature range, react 1-2h, stop logical nitrogen, be cooled to room temperature.Product is taken out, cut into fritter, in 40 DEG C of-60 DEG C of baking ovens, dry, originally execute routine prepared High hydrophilous resin water regain and reach 905g/g.
Embodiment 10: weigh 11.65g potassium hydroxide, be dissolved in 25.00ml deionized water, in the above-mentioned potassium oxide solution of the cooling lower use of ice-water bath and (28.60ml) vinylformic acid of 30.00g.Take 5.00g hydrogen peroxide oxidation yam starch, 30.00g acrylamide, 5.00mg N, N ＇-methylene-bisacrylamide, measure 35.0ml deionized water, all join in reactor, and pour the vinylformic acid having made and potassium salt soln thereof into reactor, under room temperature, stir 1.0h, it is mixed.Under the protection of nitrogen, stir, heat, control rate of heating simultaneously, bath temperature is slowly raise, graft copolymerization is fully carried out, after temperature reaches 53 DEG C, stop stirring.After this slowly heat up gradually, when after the water boiling in water-bath, continue heating and make it in this temperature range, react 1-2h, stop logical nitrogen, be cooled to room temperature.Product is taken out, cut into fritter, in 40 DEG C of-60 DEG C of baking ovens, dry, originally execute routine prepared High hydrophilous resin water regain and reach 510g/g.
Claims (4)
1. the method for High hydrophilous resin is prepared in the copolymerization of hydrogen peroxide oxidation potato starch graft, is characterised in that its method and step are: hydrogen peroxide oxidation yam starch is mixed by the mass ratio of 1:4～6 with deionized water; Take the vinylformic acid of 2～10 times of hydrogen peroxide oxidation yam starch quality, take vinylformic acid quality 0.111-0.333 sodium hydroxide (or vinylformic acid quality 0.156-0.467 potassium hydroxide doubly) doubly, with the above-mentioned sodium hydroxide of deionized water dissolving (or potassium hydroxide) of 4～6 times of hydrogen peroxide oxidation yam starch quality; In the ice-water bath above-mentioned sodium hydroxide of cooling lower use (or potassium hydroxide) solution and vinylformic acid, take vinylformic acid quality 0.5-3 acrylamide doubly.
By above-mentioned hydrogen peroxide oxidation yam starch and the mixed solution of deionized water with mix in reaction vessel with acrylic acid solution and the acrylamide of the neutralization of sodium hydroxide (or potassium hydroxide) part, without additional initiator, add the N that contains hydrogen peroxide oxidation yam starch quality 0.02～0.18%, N ＇-methylene-bisacrylamide solution makees linking agent, it is even that stirring makes it, pass into nitrogen, slowly heating, temperature of reaction system is progressively raise, reaching 50 DEG C stops stirring, 90 DEG C of insulations were taken out product after one hour, drying, pulverize and obtain High hydrophilous resin.
3. best product 1g high water absorption in the deionized water of 7000 times reaches 2000g/g.
4. described above, in the present invention, be sodium hydroxide or potassium hydroxide with vinylformic acid alkali used, N, the concentration of N ＇-methylene-bisacrylamide solution is 2mg/ml.
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| CN105713141A (en) * | 2015-05-20 | 2016-06-29 | 内蒙古大学 | Method for preparing high-nitrogen-content, high-potassium-content and high-water-absorption resin by using carboxymethyl potato starch and hydrogen peroxide as raw materials by one-pot method |
| CN105936660A (en) * | 2016-06-28 | 2016-09-14 | 内蒙古大学 | Method taking carboxymethyl potato starch as raw materials to synthesize Pb<2+> adsorption resin |
| CN106008829A (en) * | 2016-06-28 | 2016-10-12 | 内蒙古大学 | Method for preparing Co<2+> ion adsorption resin through one-pot oxidation, alkali gelatinization and graft polymerization by taking potato starch as raw material |
| CN106008827A (en) * | 2016-06-28 | 2016-10-12 | 内蒙古大学 | Method for preparing Mg<2+> ion adsorption resin through one-pot oxidation, alkali gelatinization and graft polymerization by taking potato starch as raw material |
| CN106008838A (en) * | 2016-06-28 | 2016-10-12 | 内蒙古大学 | Method for synthesizing potassium-containing super absorbent resin through one-pot graft polymerization by taking potato starch as raw material |
| CN106046261A (en) * | 2016-06-28 | 2016-10-26 | 内蒙古大学 | Method for synthesizing super absorbent resin containing potassium and nitrogen through one-pot graft copolymerization with potato starch as raw material |
| CN106046260A (en) * | 2016-06-28 | 2016-10-26 | 内蒙古大学 | Method for preparing Pb<2+> ion adsorbing resin from potato starch by oxidation/alkali gelatinization/graft polymerization one-pot process |
| CN106084134A (en) * | 2016-06-28 | 2016-11-09 | 内蒙古大学 | The method being raw material one kettle way graft copolymerization synthesis High hydrophilous resin with potato starch |
| CN106117441A (en) * | 2016-06-28 | 2016-11-16 | 内蒙古大学 | The method being raw material one kettle way glycerol polymerization synthesizing super absorbent resin with potato starch |
| CN106146737A (en) * | 2015-05-20 | 2016-11-23 | 内蒙古大学 | The method preparing super absorbent resin with high potassium content for raw material one kettle way with carboxymethyl potato starch and hydrogen peroxide |
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| CN105713141A (en) * | 2015-05-20 | 2016-06-29 | 内蒙古大学 | Method for preparing high-nitrogen-content, high-potassium-content and high-water-absorption resin by using carboxymethyl potato starch and hydrogen peroxide as raw materials by one-pot method |
| CN106146737A (en) * | 2015-05-20 | 2016-11-23 | 内蒙古大学 | The method preparing super absorbent resin with high potassium content for raw material one kettle way with carboxymethyl potato starch and hydrogen peroxide |
| CN105713141B (en) * | 2015-05-20 | 2021-04-27 | 内蒙古大学 | Method for preparing high-nitrogen and high-potassium-content high-water-absorption resin by taking carboxymethyl potato starch and hydrogen peroxide as raw materials through one-pot method |
| CN105936660A (en) * | 2016-06-28 | 2016-09-14 | 内蒙古大学 | Method taking carboxymethyl potato starch as raw materials to synthesize Pb<2+> adsorption resin |
| CN106008829A (en) * | 2016-06-28 | 2016-10-12 | 内蒙古大学 | Method for preparing Co<2+> ion adsorption resin through one-pot oxidation, alkali gelatinization and graft polymerization by taking potato starch as raw material |
| CN106008827A (en) * | 2016-06-28 | 2016-10-12 | 内蒙古大学 | Method for preparing Mg<2+> ion adsorption resin through one-pot oxidation, alkali gelatinization and graft polymerization by taking potato starch as raw material |
| CN106008838A (en) * | 2016-06-28 | 2016-10-12 | 内蒙古大学 | Method for synthesizing potassium-containing super absorbent resin through one-pot graft polymerization by taking potato starch as raw material |
| CN106046261A (en) * | 2016-06-28 | 2016-10-26 | 内蒙古大学 | Method for synthesizing super absorbent resin containing potassium and nitrogen through one-pot graft copolymerization with potato starch as raw material |
| CN106046260A (en) * | 2016-06-28 | 2016-10-26 | 内蒙古大学 | Method for preparing Pb<2+> ion adsorbing resin from potato starch by oxidation/alkali gelatinization/graft polymerization one-pot process |
| CN106084134A (en) * | 2016-06-28 | 2016-11-09 | 内蒙古大学 | The method being raw material one kettle way graft copolymerization synthesis High hydrophilous resin with potato starch |
| CN106117441A (en) * | 2016-06-28 | 2016-11-16 | 内蒙古大学 | The method being raw material one kettle way glycerol polymerization synthesizing super absorbent resin with potato starch |
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