CN101935379B - Method for synthesizing nitrogenous super absorbent resin from alkaline gelatinized potato starch through graft copolymerization - Google Patents
Method for synthesizing nitrogenous super absorbent resin from alkaline gelatinized potato starch through graft copolymerization Download PDFInfo
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Abstract
The present invention discloses a new process for synthesizing super absorbent resin, which mainly comprises the following steps of: preparing strong alkaline solution with a certain concentration, and dropwise adding the strong alkaline solution into potato starch milk at room temperature to prepare alkaline gelatinized potato starch; heating in water bath under the protection of nitrogen gas so that the graft copolymerization reaction between the alkaline gelatinized potato starch and crylic acid, sodium acrylate and acrylamide occurs to prepare nitrogenous super absorbent resin. The prepared nitrogenous super absorbent resin has good liquid absorption capability, and the highest absorption quantity of deionized water is 1200-1500 times. The potato starch milk is gelatinized by completely using the strong alkaline solution at room temperature, and the prepared alkaline gelatinized potato starch is used for synthesizing the nitrogenous super absorbent resin for the first time. Compared with other preparation methods of super absorbent resin, the method has simple process, low energy consumption and easy operation and control, and a new approach is developed for the mass production of super absorbent resin in future.
Description
Technical field
The present invention relates to a kind of synthetic method that is used for the new functional macromolecule material-High hydrophilous resin in fields such as agricultural, forestry, livestock industry, gardening, referring in particular to yam starch, vinylformic acid, acrylamide, sodium hydroxide is a kind of novel simple method for preparing of the synthetic nitrogenous High hydrophilous resin of main raw material.
Background technology
Water-absorbent that High hydrophilous resin is good and water-retentivity make it all obtain application in a lot of fields.High hydrophilous resin is joined in the soil, can change the crumb structure of soil, increase water-permeable, the ventilation property of soil, and the water that adds can be stored, have tempting prospect at aspects such as the moisture maintenance of arid area soil, desert controls.This series products has been widely used in fields such as seed pelleting, desertification treatment, agricultural gardening at present, and its demand is with very high speed increment.
The preparation method of High hydrophilous resin is a lot, and synthesis material is abundant, and production technique is different.Though China is obtaining certain achievement aspect the research of High hydrophilous resin, but the product of industrialization is also existing many problems aspect performance and the kind, suction multiple as resin is low, salt resistant character is poor, low, the complex manufacturing of gel-strength, product cost after the suction are high, and it is also few in the research of suction theory, water absorbing properties and application facet, the kind of suitability for industrialized production manufacturer production and quantity are also fewer, have many need of work people deeply to do.We should give full play to the abundant advantage of China's yam starch natural resource, produce the High hydrophilous resin of high-quality suitable China's national situation, lay the foundation for High hydrophilous resin becomes the third-largest agrochemicals of China and is applied to every field.
The High hydrophilous resin water-absorbent is extremely strong, and its suction back swelling is a gel, and when being subjected to the external force extruding, water also is difficult for running off, and has good water retention property.High hydrophilous resin is born in the sixties in 20th century as a kind of novel functional high molecule material, at present, is that the development of raw material synthetic High hydrophilous resin is very fast with starch.
Starch is one of raw material of synthesizing super absorbent resin preferably, and it is a kind of natural high moleculer eompound of renewable, wide material sources.The graft polymerization or the multipolymer of wetting ability vinyl monomers such as starch and vinyl cyanide, vinylformic acid, acrylamide are one of principal item in the present High hydrophilous resin market.Because starch is cheap, biodegradability good, other synthesizing series has remarkable advantages relatively on market, and have advantages such as suction multiple height, absorption speed be fast, so be that raw material synthetic High hydrophilous resin has more wide application prospect with the yam starch with the High hydrophilous resin of yam starch preparation.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of novel method of synthesizing super absorbent resin, this preparation method is with yam starch, vinylformic acid, acrylamide, sodium hydroxide, Potassium Persulphate, N, N '-methylene-bisacrylamide is a main raw material, makes nitrogenous High hydrophilous resin through reasonable proportioning, simple synthetic route.
The technical problem to be solved in the present invention is solved by following scheme: the method for the synthetic nitrogenous High hydrophilous resin of alkali pasting potato starch graft copolymer, it is characterized in that: compound concentration is the N of 2mg/ml, N '-methylene-bisacrylamide solution 0.8-1.4ml, wherein yam starch and N, the mass ratio of N '-methylene-bisacrylamide is 1: 0.0016-0.0028; Yam starch mixes with the mass ratio of deionized water with 1: 3, stir 0.5-1.0h, preparation hydroxide radical volumetric molar concentration is the strong base solution of 0.550-0.700mol/L, wherein yam starch and alkaline mass ratio are 1: 0.044-0.078, at room temperature with the fast pasting potato starch milk that drips of 10-15 second/drip, make alkali pasting potato starch with the strong base solution for preparing; Under the ice-water bath cooling, remove the vinylformic acid of stopper with the sodium hydroxide solution neutralization, obtain vinylformic acid and sodium salt solution thereof that the vinylformic acid degree of neutralization is 30%-80%, wherein the mass ratio of the deionized water of yam starch and vinylformic acid, sodium hydroxide, dissolved hydrogen sodium oxide is 1: 3-7: 0.500-3.108: 5; The preparation acrylamide soln, wherein the mass ratio of the deionized water of yam starch and acrylamide, dissolving acrylamide is 1: 0.5-2.5: 3; The alkali pasting potato starch that makes and vinylformic acid and sodium salt solution thereof, acrylamide soln are mixed, add deionized water simultaneously, wherein yam starch is 1 with the mass ratio of adding deionized water: 0-4.754, the Potassium Persulphate that adds yam starch quality 1.4-1.8% is made initiator, adding concentration is the N of 2mg/ml, N '-methylene-bisacrylamide solution 0.8-1.4ml makees linking agent, stirs 0.5-1.0h under the room temperature, and it is mixed; Under nitrogen protection, heating in water bath makes alkali pasting potato starch and vinylformic acid and sodium salt thereof, acrylamide carry out graft copolymerization; and make reactant under the boiling water bath heating, be incubated 1.0-2.0h; product is taken out, and oven dry is also pulverized, and promptly gets nitrogenous High hydrophilous resin.The highest suction amount of deionized water of prepared nitrogenous High hydrophilous resin is 1200-1400g/g.
Technique scheme is described, and used highly basic was sodium hydroxide, potassium hydroxide when preparation hydroxide radical volumetric molar concentration was the strong base solution of 0.550-0.700mol/L, preferred sodium hydroxide.
Technique scheme is described, and the vinylformic acid degree of neutralization of prepared High hydrophilous resin is 30%-80%, and its degree of neutralization is 30%, 40%, and 50%, 60%, 65%, 70%, 80%.The preferred 40%-80% of degree of neutralization, most preferably 60%-80%.
Technique scheme is described, and the purpose of adding deionized water is: except the volume of cross-linking agent solution, for the cumulative volume that makes reaction system is consistent.Except the deionized water of adding, dissolving alkaline deionized water when other liquid comprises the alkali gelatinization in the reaction system, in and the deionized water of deionized water, the deionized water that disperses yam starch, liquid acrylic and the dissolving acrylamide of dissolved hydrogen sodium oxide during vinylformic acid.
Advantage of the present invention is: 1, patent of the present invention is at room temperature carried out gelatinization to the yam starch breast with strong base solution fully, and carry out the synthetic of nitrogenous High hydrophilous resin with this alkali pasting potato starch that makes first, the imbibition ability of final prepared nitrogenous High hydrophilous resin is better, and its highest suction amount of deionized water at 1200-1400 doubly.2, be in the process of parent synthesizing super absorbent resin with starch, at first all starch to be heated gelatinization, carry out the synthetic High hydrophilous resin of graft copolymerization with monomer again, but the hot gelatinization of starch mainly contains following shortcoming: (1) but the heating gelatinization need expend very big heat makes just starch solution generation gelatinization reaction, and need certain gelatinization time, the gelatinization point of general starch is 50 ℃-80 ℃; (2) gelatinization point should not be controlled, and the too high meeting of temperature causes starch " to wear out ", is difficult for disperseing in water, and percentage of grafting is reduced, and water-retaining capacity descends, and temperature is crossed low then starch the gelatinization effect is not taken place; (3) gelatinization point of the starch of different types of starch and different production batchs all can have difference, and the gelatinization point to starch requires very strict when being the raw material synthesizing super absorbent resin with hot pasted starch, this is just for scale operation has caused very large unfavorable factor, and water regain instability, the poor repeatability of institute's synthetic High hydrophilous resin.In the patent of the present invention, adopt strong base solution at room temperature yam starch to be carried out gelatinization and be the novel process of raw material synthesizing super absorbent resin with the yam starch after the alkali gelatinization, overcome above shortcoming when being the raw material synthesizing super absorbent resin with hot pasted starch, at first, the alkali gelatinization need not heating, gelatinization time is very short, at room temperature can finish reaction, not need to expend heat energy; Secondly, only need strong base solution is added drop-wise to the yam starch Ruzhong, and control the gelatinization that rate of addition can be finished yam starch, this is more intuitively easier than controlled temperature, is more conducive to large-scale production, has beyond thought technique effect.3, the raw material of producing this product is a yam starch, and it is the very large agricultural-food of the northern area of China output, and the promotion conference of this product expands out a new road for the deep processing of the northern area of China agricultural-food, and the peasant is increased income.
Description of drawings
Fig. 1 is the process flow sheet of the nitrogenous High hydrophilous resin of preparation
Sodium hydroxide concentration was inhaled the influence curve of amount of deionized water when Fig. 2 was the alkali gelatinization to product
Fig. 3 is the acrylamide consumption is inhaled amount of deionized water to product a influence curve
Fig. 4 is the vinylformic acid consumption is inhaled amount of deionized water to product a influence curve
Fig. 5 is acrylic acid degree of neutralization is inhaled amount of deionized water to product a influence curve
Fig. 6 is dosage of crosslinking agent is inhaled amount of deionized water to product a influence curve
Fig. 7 is initiator amount is inhaled amount of deionized water to product a influence curve
Embodiment
Embodiment 1: take by weighing 0.24g sodium hydroxide, be dissolved in the 10.0ml deionized water, be mixed with the sodium hydroxide solution that the hydroxide radical volumetric molar concentration is 0.600mol/L; Take by weighing 8.3g sodium hydroxide, be dissolved in the 25.0ml deionized water, be mixed with sodium hydroxide solution, under ice-water bath cooling and stirring condition, in and 30.0g (28.52ml) remove the vinylformic acid of stopper, make acrylic acid degree of neutralization and be 50% vinylformic acid and sodium salt solution thereof; Take by weighing the 5.0g yam starch, mix with the 15.0ml deionized water, stir 0.5h after, be that the sodium hydroxide solution of 0.600mol/L is with 10-15 with the hydroxide radical volumetric molar concentration
Second/dripDrip fast pasting potato starch milk; Take by weighing the 10g acrylamide, be dissolved in the 15ml deionized water; The alkali pasting potato starch that makes and vinylformic acid and sodium salt solution thereof, acrylamide soln are mixed, add the 14.3ml deionized water, adding 80mg Potassium Persulphate, 5ml concentration are the N of 2mg/ml, N '-methylene-bisacrylamide solution, under room temperature, stir 0.5h, it is mixed; Heating in water bath heats up gradually under the condition of nitrogen protection; make alkali pasting potato starch and vinylformic acid and sodium salt thereof, acrylamide carry out graft copolymerization, and make product in boiling water bath, be incubated 1.0-2.0h, product is taken out; oven dry is also pulverized, and promptly gets nitrogenous High hydrophilous resin.It is 780g/g that the prepared nitrogenous High hydrophilous resin of present embodiment is inhaled amount of deionized water.
Embodiment 2: experiment condition is with embodiment 1, that different is weighing sodium hydroxide 0.22g, be dissolved in the 10.0ml deionized water, preparation hydroxide radical volumetric molar concentration is the sodium hydroxide solution of 0.550mol/L, and it is 595g/g that the prepared nitrogenous High hydrophilous resin of present embodiment is inhaled amount of deionized water.
Embodiment 3: experiment condition is with embodiment 1, that different is weighing sodium hydroxide 0.23g, be dissolved in the 10.0ml deionized water, preparation hydroxide radical volumetric molar concentration is the sodium hydroxide solution of 0.575mol/L, and it is 720g/g that the prepared nitrogenous High hydrophilous resin of present embodiment is inhaled amount of deionized water.
Embodiment 4: experiment condition is with embodiment 1, that different is weighing sodium hydroxide 0.25g, be dissolved in the 10.0ml deionized water, preparation hydroxide radical volumetric molar concentration is the sodium hydroxide solution of 0.625mol/L, and it is 660g/g that the prepared nitrogenous High hydrophilous resin of present embodiment is inhaled amount of deionized water.
Embodiment 5: experiment condition is with embodiment 1, that different is weighing sodium hydroxide 0.26g, be dissolved in the 10.0ml deionized water, preparation hydroxide radical volumetric molar concentration is the sodium hydroxide solution of 0.650mol/L, and it is 650g/g that the prepared nitrogenous High hydrophilous resin of present embodiment is inhaled amount of deionized water.
Embodiment 6: experiment condition is with embodiment 1, that different is weighing sodium hydroxide 0.27g, be dissolved in the 10.0ml deionized water, preparation hydroxide radical volumetric molar concentration is the sodium hydroxide solution of 0.675mol/L, and it is 625g/g that the prepared nitrogenous High hydrophilous resin of present embodiment is inhaled amount of deionized water.
Embodiment 7: experiment condition is with embodiment 1, and different is to take by weighing the 2.5g acrylamide, is dissolved in the 15ml deionized water, and it is 1340g/g that the prepared nitrogenous High hydrophilous resin of present embodiment is inhaled amount of deionized water.
Embodiment 8: experiment condition is with embodiment 1, and different is to take by weighing the 5.0g acrylamide, is dissolved in the 15ml deionized water, and it is 1135g/g that the prepared nitrogenous High hydrophilous resin of present embodiment is inhaled amount of deionized water.
Embodiment 9: experiment condition is with embodiment 1, and different is to take by weighing the 7.5g acrylamide, is dissolved in the 15ml deionized water, and it is 900g/g that the prepared nitrogenous High hydrophilous resin of present embodiment is inhaled amount of deionized water.
Embodiment 10: experiment condition is with embodiment 1, and different is to take by weighing the 12.5g acrylamide, is dissolved in the 15ml deionized water, and it is 550g/g that the prepared nitrogenous High hydrophilous resin of present embodiment is inhaled amount of deionized water.
Embodiment 11: experiment condition is with embodiment 1, different is to take by weighing 4.2g sodium hydroxide, be dissolved in the 25.0ml deionized water, be mixed with sodium hydroxide solution, under ice-water bath cooling and stirring condition, in and 15.0g (14.26ml) remove the vinylformic acid of stopper, make acrylic acid degree of neutralization and be 50% vinylformic acid and sodium salt solution thereof; Take by weighing the 5.0g acrylamide, be dissolved in the 15ml deionized water, it is 810g/g that the prepared nitrogenous High hydrophilous resin of present embodiment is inhaled amount of deionized water.
Embodiment 12: experiment condition is with embodiment 1, different is to take by weighing 5.6g sodium hydroxide, be dissolved in the 25.0ml deionized water, be mixed with sodium hydroxide solution, under ice-water bath cooling and stirring condition, in and 20.0g (19.01ml) remove the vinylformic acid of stopper, make acrylic acid degree of neutralization and be 50% vinylformic acid and sodium salt solution thereof; Take by weighing the 5.0g acrylamide, be dissolved in the 15ml deionized water, it is 840g/g that the prepared nitrogenous High hydrophilous resin of present embodiment is inhaled amount of deionized water.
Embodiment 13: experiment condition is with embodiment 1, different is to take by weighing 6.9g sodium hydroxide, be dissolved in the 25.0ml deionized water, be mixed with sodium hydroxide solution, under ice-water bath cooling and stirring condition, in and 25.0g (23.76ml) remove the vinylformic acid of stopper, make acrylic acid degree of neutralization and be 50% vinylformic acid and sodium salt solution thereof; Take by weighing the 5.0g acrylamide, be dissolved in the 15ml deionized water, it is 890g/g that the prepared nitrogenous High hydrophilous resin of present embodiment is inhaled amount of deionized water.
Embodiment 14: experiment condition is with embodiment 1, different is to take by weighing 11.1g sodium hydroxide, be dissolved in the 25.0ml deionized water, be mixed with sodium hydroxide solution, under ice-water bath cooling and stirring condition, in and 35.0g (33.27ml) remove the vinylformic acid of stopper, make acrylic acid degree of neutralization and be 50% vinylformic acid and sodium salt solution thereof; Take by weighing the 5.0g acrylamide, be dissolved in the 15ml deionized water, it is 820g/g that the prepared nitrogenous High hydrophilous resin of present embodiment is inhaled amount of deionized water.
Embodiment 15: experiment condition is with embodiment 1, different is to take by weighing 5.0g sodium hydroxide, be dissolved in the 25.0ml deionized water, be mixed with sodium hydroxide solution, under ice-water bath cooling and stirring condition, in and 30.0g (28.52ml) remove the vinylformic acid of stopper, make acrylic acid degree of neutralization and be 30% vinylformic acid and sodium salt solution thereof, take by weighing the 5.0g acrylamide, be dissolved in the 15ml deionized water, it is 890g/g that the prepared nitrogenous High hydrophilous resin of present embodiment is inhaled amount of deionized water.
Embodiment 16: experiment condition is with embodiment 1, different is to take by weighing 6.7g sodium hydroxide, be dissolved in the 25.0ml deionized water, be mixed with sodium hydroxide solution, under ice-water bath cooling and stirring condition, in and 30.0g (28.52ml) remove the vinylformic acid of stopper, make acrylic acid degree of neutralization and be 40% vinylformic acid and sodium salt solution thereof, take by weighing the 5.0g acrylamide, be dissolved in the 15ml deionized water, it is 1020g/g that the prepared nitrogenous High hydrophilous resin of present embodiment is inhaled amount of deionized water.
Embodiment 17: experiment condition is with embodiment 1, different is to take by weighing 10.0g sodium hydroxide, be dissolved in the 25.0ml deionized water, be mixed with sodium hydroxide solution, under ice-water bath cooling and stirring condition, in and 30.0g (28.52ml) remove the vinylformic acid of stopper, make acrylic acid degree of neutralization and be 60% vinylformic acid and sodium salt solution thereof, take by weighing the 5.0g acrylamide, be dissolved in the 15ml deionized water, it is 1270g/g that the prepared nitrogenous High hydrophilous resin of present embodiment is inhaled amount of deionized water.
Embodiment 18: experiment condition is with embodiment 1, different is to take by weighing 10.8g sodium hydroxide, be dissolved in the 25.0ml deionized water, be mixed with sodium hydroxide solution, under ice-water bath cooling and stirring condition, in and 30.0g (28.52ml) remove the vinylformic acid of stopper, make acrylic acid degree of neutralization and be 65% vinylformic acid and sodium salt solution thereof, take by weighing the 5.0g acrylamide, be dissolved in the 15ml deionized water, it is 1400g/g that the prepared nitrogenous High hydrophilous resin of present embodiment is inhaled amount of deionized water.
Embodiment 19: experiment condition is with embodiment 1, different is to take by weighing 11.7g sodium hydroxide, be dissolved in the 25.0ml deionized water, be mixed with sodium hydroxide solution, under ice-water bath cooling and stirring condition, in and 30.0g (28.52ml) remove the vinylformic acid of stopper, make acrylic acid degree of neutralization and be 70% vinylformic acid and sodium salt solution thereof, take by weighing the 5.0g acrylamide, be dissolved in the 15ml deionized water, it is 1270g/g that the prepared nitrogenous High hydrophilous resin of present embodiment is inhaled amount of deionized water.
Embodiment 20: experiment condition is with embodiment 1, different is to take by weighing 13.3g sodium hydroxide, be dissolved in the 25.0ml deionized water, be mixed with sodium hydroxide solution, under ice-water bath cooling and stirring condition, in and 30.0g (28.52ml) remove the vinylformic acid of stopper, make acrylic acid degree of neutralization and be 80% vinylformic acid and sodium salt solution thereof, take by weighing the 5.0g acrylamide, be dissolved in the 15ml deionized water, it is 1240g/g that the prepared nitrogenous High hydrophilous resin of present embodiment is inhaled amount of deionized water.
Embodiment 21: experiment condition is with embodiment 1, different is to take by weighing 10.8g sodium hydroxide, be dissolved in the 25.0ml deionized water, be mixed with sodium hydroxide solution, under ice-water bath cooling and stirring condition, in and 30.0g (28.52ml) remove the vinylformic acid of stopper, make acrylic acid degree of neutralization and be 65% vinylformic acid and sodium salt solution thereof, take by weighing the 5.0g acrylamide, be dissolved in the 15ml deionized water, adding 4ml concentration is the N of 2mg/ml, N '-methylene-bisacrylamide solution, and it is 860g/g that the prepared nitrogenous High hydrophilous resin of present embodiment is inhaled amount of deionized water.
Embodiment 22: experiment condition is with embodiment 1, different is to take by weighing 10.8g sodium hydroxide, be dissolved in the 25.0ml deionized water, be mixed with sodium hydroxide solution, under ice-water bath cooling and stirring condition, in and 30.0g (28.52ml) remove the vinylformic acid of stopper, make acrylic acid degree of neutralization and be 65% vinylformic acid and sodium salt solution thereof, take by weighing the 5.0g acrylamide, be dissolved in the 15ml deionized water, adding 5.5ml concentration is the N of 2mg/ml, N '-methylene-bisacrylamide solution, and it is 1030g/g that the prepared nitrogenous High hydrophilous resin of present embodiment is inhaled amount of deionized water.
Embodiment 23: experiment condition is with embodiment 1, different is to take by weighing 10.8g sodium hydroxide, be dissolved in the 25.0ml deionized water, be mixed with sodium hydroxide solution, under ice-water bath cooling and stirring condition, in and 30.0g (28.52ml) remove the vinylformic acid of stopper, make acrylic acid degree of neutralization and be 65% vinylformic acid and sodium salt solution thereof, take by weighing the 5.0g acrylamide, be dissolved in the 15ml deionized water, adding 6ml concentration is the N of 2mg/ml, N '-methylene-bisacrylamide solution, and it is 970g/g that the prepared nitrogenous High hydrophilous resin of present embodiment is inhaled amount of deionized water.
Embodiment 24: experiment condition is with embodiment 1, different is to take by weighing 10.8g sodium hydroxide, be dissolved in the 25.0ml deionized water, be mixed with sodium hydroxide solution, under ice-water bath cooling and stirring condition, in and 30.0g (28.52ml) remove the vinylformic acid of stopper, make acrylic acid degree of neutralization and be 65% vinylformic acid and sodium salt solution thereof, take by weighing the 5.0g acrylamide, be dissolved in the 15ml deionized water, adding 7ml concentration is the N of 2mg/ml, N '-methylene-bisacrylamide solution, and it is 920g/g that the prepared nitrogenous High hydrophilous resin of present embodiment is inhaled amount of deionized water.
Embodiment 25: experiment condition is with embodiment 1, different is to take by weighing 10.8g sodium hydroxide, be dissolved in the 25.0ml deionized water, be mixed with sodium hydroxide solution, under ice-water bath cooling and stirring condition, in and 30.0g (28.52ml) remove the vinylformic acid of stopper, make acrylic acid degree of neutralization and be 65% vinylformic acid and sodium salt solution thereof, take by weighing the 5.0g acrylamide, be dissolved in the 15ml deionized water, add the 70mg Potassium Persulphate, it is 800g/g that the prepared nitrogenous High hydrophilous resin of present embodiment is inhaled amount of deionized water.
Embodiment 26: experiment condition is with embodiment 1, different is to take by weighing 10.8g sodium hydroxide, be dissolved in the 25.0ml deionized water, be mixed with sodium hydroxide solution, under ice-water bath cooling and stirring condition, in and 30.0g (28.52ml) remove the vinylformic acid of stopper, make acrylic acid degree of neutralization and be 65% vinylformic acid and sodium salt solution thereof, take by weighing the 5.0g acrylamide, be dissolved in the 15ml deionized water, add the 75mg Potassium Persulphate, it is 830g/g that the prepared nitrogenous High hydrophilous resin of present embodiment is inhaled amount of deionized water.
Embodiment 27: experiment condition is with embodiment 1, different is to take by weighing 10.8g sodium hydroxide, be dissolved in the 25.0ml deionized water, be mixed with sodium hydroxide solution, under ice-water bath cooling and stirring condition, in and 30.0g (28.52ml) remove the vinylformic acid of stopper, make acrylic acid degree of neutralization and be 65% vinylformic acid and sodium salt solution thereof, take by weighing the 5.0g acrylamide, be dissolved in the 15ml deionized water, add the 85mg Potassium Persulphate, it is 1080g/g that the prepared nitrogenous High hydrophilous resin of present embodiment is inhaled amount of deionized water.
Embodiment 28: experiment condition is with embodiment 1, different is to take by weighing 10.8g sodium hydroxide, be dissolved in the 25.0ml deionized water, be mixed with sodium hydroxide solution, under ice-water bath cooling and stirring condition, in and 30.0g (28.52ml) remove the vinylformic acid of stopper, make acrylic acid degree of neutralization and be 65% vinylformic acid and sodium salt solution thereof, take by weighing the 5.0g acrylamide, be dissolved in the 15ml deionized water, add the 90mg Potassium Persulphate, it is 970g/g that the prepared nitrogenous High hydrophilous resin of present embodiment is inhaled amount of deionized water.
Claims (4)
1. alkali pasting potato starch graft copolymer synthesizes the method for nitrogenous High hydrophilous resin, it is characterized in that: compound concentration is the N of 2mg/ml, N ＇-methylene-bisacrylamide solution 0.8-1.4ml, wherein yam starch and N, the mass ratio of N ＇-methylene-bisacrylamide is 1: 0.0016-0.0028; Yam starch mixes with the mass ratio of deionized water with 1: 3, stir 0.5-1.0h, preparation hydroxide radical volumetric molar concentration is the strong base solution of 0.550-0.700mol/L, wherein yam starch and alkaline mass ratio are 1: 0.044-0.078, at room temperature with the fast pasting potato starch milk that drips of 10-15 second/drip, make alkali pasting potato starch with the strong base solution for preparing; Under the ice-water bath cooling, remove the vinylformic acid of stopper with the sodium hydroxide solution neutralization, obtain vinylformic acid and sodium salt solution thereof that acrylic acid degree of neutralization is 30%-80%, wherein the mass ratio of the deionized water of yam starch and vinylformic acid, sodium hydroxide, dissolved hydrogen sodium oxide is 1: 3-7: 0.500-3.108: 5; The preparation acrylamide soln, wherein the mass ratio of yam starch and acrylamide, dissolving acrylamide deionized water is 1: 0.5-2.5: 3; The alkali pasting potato starch that makes and vinylformic acid and sodium salt solution thereof, acrylamide soln are mixed, add deionized water simultaneously, wherein yam starch is 1 with the mass ratio of adding deionized water: 0-4.754, the Potassium Persulphate that adds yam starch quality 1.4-1.8% is made initiator, adding concentration is the N of 2mg/ml, N ＇-methylene-bisacrylamide solution 0.8-1.4ml makees linking agent, stirs 0.5-1.0h under the room temperature, and it is mixed; Under nitrogen protection; heating in water bath; make alkali pasting potato starch and vinylformic acid and sodium salt thereof, acrylamide carry out graft copolymerization; and make product in boiling water bath, be incubated 1.0-2.0h; product is taken out; oven dry is also pulverized, and promptly gets nitrogenous High hydrophilous resin, and the highest suction amount of deionized water of prepared nitrogenous High hydrophilous resin is 1200-1400g/g.
2. according to the method for the synthetic nitrogenous High hydrophilous resin of the described alkali pasting potato of claim 1 starch graft copolymer, it is characterized in that: used highly basic was sodium hydroxide, potassium hydroxide when preparation hydroxide radical volumetric molar concentration was the strong base solution of 0.550-0.700mol/L.
3. according to the method for the synthetic nitrogenous High hydrophilous resin of the described alkali pasting potato of claim 1 starch graft copolymer, it is characterized in that: used highly basic was sodium hydroxide when preparation hydroxide radical volumetric molar concentration was the strong base solution of 0.550-0.700mol/L.
4. according to the method for the synthetic nitrogenous High hydrophilous resin of the described alkali pasting potato of claim 1 starch graft copolymer, it is characterized in that: acrylic acid degree of neutralization of obtained High hydrophilous resin is 40%-80%.
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| CN108948271B (en) * | 2018-08-31 | 2021-03-02 | 昆明理工大学 | Preparation method and application of potato residue treating agent |
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