CN106046261A - Method for synthesizing super absorbent resin containing potassium and nitrogen through one-pot graft copolymerization with potato starch as raw material - Google Patents
Method for synthesizing super absorbent resin containing potassium and nitrogen through one-pot graft copolymerization with potato starch as raw material Download PDFInfo
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- CN106046261A CN106046261A CN201610481266.1A CN201610481266A CN106046261A CN 106046261 A CN106046261 A CN 106046261A CN 201610481266 A CN201610481266 A CN 201610481266A CN 106046261 A CN106046261 A CN 106046261A
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- potato starch
- potassium
- nitrogen
- acrylamide
- water
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B31/00—Preparation of derivatives of starch
- C08B31/18—Oxidised starch
Abstract
The invention discloses a method for preparing super absorbent resin containing potassium and nitrogen through one-pot graft copolymerization with potato starch as a raw material. The method is mainly characterized in that the potato starch is oxidized by 30% hydrogen peroxide, then acrylic acid and potassium salt thereof with a polymerization inhibitor removed and acrylamide are used for synthesizing the super absorbent resin containing potassium and nitrogen by adopting a one-pot process under nitrogen protection and water-bath heating conditions, and the highest water absorption of the best product in 5000 times of deionized water can reach 950g/g. The method for preparing the super absorbent resin has the advantages that the potato starch is oxidized by hydrogen peroxide, and the traditional separation, purification and washing carried out on oxidized potato starch are not needed; an initiating agent does not need to be added when the super absorbent resin is synthesized, and the obtained product has relatively high water absorption and contains nitrogen and potassium elements, so that the super absorbent resin synthesis technology is simple, cost is low, and the product has excellent performance, is especially high in water absorption and contains the nitrogen and potassium elements, is a good dual-purpose product applied to agriculture and horticulture and has good application and popularization values.
Description
Technical field
The present invention relates to the water suction of a kind of functional high molecule material height for the field such as industry, agricultural, desertification treatment
The preparation method of resin, it is main for particularly relating to potato starch, hydrogen peroxide, acrylic acid, potassium hydroxide and acrylamide
Raw material one kettle way prepares nitrogenous and potassium High hydrophilous resin method.
Background technology
Super absorbent resin is the functional high molecule material that a class is novel.Due to water suction, the water retention property of its uniqueness,
The aspects such as medical and health, agricultural gardening, desert treatment obtain a wide range of applications.Starch-series High hydrophilous resin prepare raw material
Source is extensive, synthesis technique is simple.Starch belongs to the polymer of glucose, is widely distributed in the group such as the seed of numerous plant, root block
In knitting, wide material sources, thus use starch and derivant synthesizing super absorbent polymer thereof that cost of material can be greatly lowered, with
Time prepared product there is good performance.
Research about High hydrophilous resin at present gets more and more, but water absorbent rate is the highest, complex technical process, and cost is high
The problem always making researcher puzzlement etc. problem, the polymerization of High hydrophilous resin needs the initiation of initiator, initiator mainly to have
Free radical (such as azo and persulfate etc.) initiator and redox initiator two class, but the shortcoming of this two classes initiator
It is to introduce foreign ion, eventually affects the water absorption of High hydrophilous resin.Therefore, these problems of the most just right solution
It it is current research emphasis.
The application have employed first potato starch after hydrogen peroxide oxidation directly with remove polymerization inhibitor acrylic acid and
Its potassium salt, acrylamide one pot process be nitrogenous and the method for potassium High hydrophilous resin, and traditional method is first to use hydrogen peroxide oxidation
After potato starch through separating, washing, the step such as drying first prepare oxidised potato starch, then with oxidised potato starch
Preparing nitrogenous and potassium High hydrophilous resin for raw material and monomer copolymerization, the application eliminates dividing of oxidised potato starch well
From, wash, the step such as drying, and need not additionally add initiator, the product simultaneously prepared has higher water absorption, contains
Nitrogen element and potassium element, therefore, present invention process is simple, synthesizes low cost, practical, has good application valency
Value.
Summary of the invention
The invention provides that a kind of technique is simple, synthesis low cost, water absorbing capacity are strong, nitrogenous and potassium High hydrophilous resin produces
Product and preparation method thereof.It is main for particularly relating to potato starch, hydrogen peroxide, acrylic acid, potassium hydroxide and acrylamide
Raw material one kettle way prepares nitrogenous and potassium High hydrophilous resin method.
Its method and step are as follows:
(1) mix homogeneously under potato starch being stirred by the mass ratio of 1:8 with deionized water, at 70 DEG C, add Rhizoma Solani tuber osi form sediment
Lower oxidation reaction 0.5h of the hydrogen peroxide of the 30% of opaque amount 0.1776 times, this temperature and stirring；Weigh potato quality 2.592
Potassium hydroxide again, with the deionized water dissolving of potassium hydroxide quality 1.54 times；With the hydrogen of above-mentioned preparation under ice-water bath cools down
In potassium oxide solution and the acrylic acid of potato starch quality 6.67 times.Weigh the acryloyl of potato starch quality 1.334 times
Amine, with the deionized water dissolving acrylamide of acrylamide quality 3 times.
(2) by the potato starch solution after above-mentioned oxidation with neutralize after acrylic acid and potassium salt soln and acryloyl
Amine aqueous solution is sufficiently mixed, and adds N, the N ＇-methylene-bisacrylamide containing potato starch quality 0.25% and makees cross-linking agent, holds
Continuous stirring, is passed through nitrogen, is slowly heated, and after polyreaction starts, stops stirring, is incubated 2h, drying, powder between 80-100 DEG C
Broken i.e. obtain nitrogenous and potassium High hydrophilous resin, should under the conditions of product high water absorption in the deionized water of 5000 times of synthesis be
950g/g。
Advantages of the present invention:
(1) present invention uses potato starch to be that raw material one kettle way prepares nitrogenous and potassium High hydrophilous resin first, and technique is simple, easily
In operation.
(2) without adding initiator i.e. polymerizable, impurity, low cost will not be introduced.
(3) hydrogen peroxide catabolite is water, pollution-free, and product has excellent performance simultaneously.
(4) absorbed deionized water by the product obtained by the present invention and reach as high as 950g/g, Nitrogen element and potassium in resin
Element, has good application and popularization value, is especially applicable to agricultural and gardening is the good product killed two birds with one stone.
Accompanying drawing explanation
Fig. 1 is to prepare nitrogenous and potassium High hydrophilous resin process chart with potato starch for raw material one kettle way
Fig. 2 is that the consumption of the hydrogen peroxide of 30% is to the nitrogenous and influence curve of potassium High hydrophilous resin water absorption
Fig. 3 is that the oxidizing temperature of potato starch is to the nitrogenous and influence curve of potassium High hydrophilous resin water absorption
Fig. 4 is that the oxidization time of potato starch is to the nitrogenous and influence curve of potassium High hydrophilous resin water absorption
Fig. 5 is potato starch with monomer ratio to the nitrogenous and influence curve of potassium High hydrophilous resin water absorption
Fig. 6 is that the acrylic acid mass ratio with acrylamide is to the nitrogenous and influence curve of potassium High hydrophilous resin water absorption
Fig. 7 is that acrylic acid degree of neutralization is to the nitrogenous and influence curve of potassium High hydrophilous resin water absorption
Fig. 8 is that the consumption of cross-linking agent is to the nitrogenous and influence curve of potassium High hydrophilous resin water absorption
Fig. 9 is that the total Water of reaction system is to the nitrogenous and influence curve of potassium High hydrophilous resin water absorption.
Detailed description of the invention
Embodiment 1: weigh 5g potato starch and under agitation mix homogeneously with 40mL deionized water, 70 DEG C and stirring under add
Enter 0.8mL 30% hydrogen peroxide, and this temperature and stirring under aoxidize 1.5h；Weigh 12.96g potassium hydroxide, and use 20mL
Deionized water dissolving potassium hydroxide；Ice-water bath cool down under with in the potassium hydroxide solution of described preparation and 31.7mL(33.3g)
Acrylic acid, obtain acrylic acid and potassium salt soln thereof.Weigh 6.67g acrylamide, with 20mL deionized water dissolving acrylamide,
Obtain acrylamide solution.By above-mentioned oxidised potato starch solution with neutralize after acrylic acid and potassium salt soln and propylene
Being sufficiently mixed under amide solution stirring, N, the N ＇-methylene-bisacrylamide adding 12.5mg makees cross-linking agent, continuously stirred, logical
Enter nitrogen, be slowly heated, after polyreaction starts, stop stirring, between 80-100 DEG C, be incubated 2h, drying, pulverize i.e. to obtain and contain
Nitrogen and potassium High hydrophilous resin, under the conditions of this, product high water absorption in the deionized water of 5000 times of synthesis is 950g/g.
Embodiment 2: weigh 5g potato starch and under agitation mix homogeneously with 50mL deionized water, 60 DEG C and stirring under add
Enter 0.8mL 30% hydrogen peroxide, oxidation reaction 1.5h at such a temperature；Weigh 7.78g potassium hydroxide, and with 20mL go from
Sub-dissolved hydrogen water potassium oxide；Under ice-water bath cools down with in potassium hydroxide solution and 19.1mL(20g) acrylic acid, obtain propylene
Acid and potassium salt soln thereof.Weigh 10g acrylamide, with 20mL deionized water dissolving acrylamide, obtain acrylamide solution.Will
Above-mentioned oxidised potato starch solution with neutralize after acrylic acid and potassium salt soln and acrylamide solution stirring lower fully
Mixing, N, the N ＇-methylene-bisacrylamide adding 12.5mg makees cross-linking agent, continuously stirred, is passed through nitrogen, is slowly heated, poly-
Close after reaction starts, stop stirring, between 80-100 DEG C, be incubated 2h, drying, pulverize and i.e. obtain nitrogenous and potassium High hydrophilous resin, this
Under the conditions of synthesis product high water absorption in the deionized water of 5000 times be 675g/g.
Embodiment 3: weigh 5g potato starch and under agitation mix homogeneously with 30mL deionized water, 70 DEG C and stirring under add
Enter 0.8mL 30% hydrogen peroxide, oxidation reaction 1.5h at such a temperature；Weigh 7.78g potassium hydroxide, and with 20mL go from
Sub-dissolved hydrogen water potassium oxide；Ice-water bath cool down under with in the potassium hydroxide solution of described preparation and 19.1mL(20g) propylene
Acid obtains acrylic acid and potassium salt soln thereof.Weigh 10g acrylamide, with 20mL deionized water dissolving acrylamide, obtain propylene
Amide solution.By above-mentioned oxidised potato starch solution with neutralize after acrylic acid and potassium salt soln and acrylamide solution
Being sufficiently mixed under stirring, N, the N ＇-methylene-bisacrylamide adding 12.5mg makees cross-linking agent, continuously stirred, is passed through nitrogen, slow
Slow heating, after polyreaction starts, stops stirring, is incubated 2h between 80-100 DEG C, drying, pulverizes and i.e. obtains the nitrogenous and high suction of potassium
Water-resin, under the conditions of this, product high water absorption in the deionized water of 5000 times of synthesis is 800g/g.
Embodiment 4: weigh under 5g potato starch stirs with 30mL deionized water and mix homogeneously, adds 0.8mL at 70 DEG C
30% hydrogen peroxide, this temperature and stirring under oxidation reaction 0.5h；Weigh 6.22g potassium hydroxide, and use 20mL deionization
Water dissolution；Ice-water bath cool down under with in the potassium hydroxide solution of described preparation and 19.1mL(20g) acrylic acid obtain propylene
Acid and potassium salt soln thereof.Weigh 10g acrylamide, with 20mL deionized water dissolving acrylamide, obtain acrylamide solution.Will
Above-mentioned oxidised potato starch solution with neutralize after acrylic acid and potassium salt soln and acrylamide solution stirring lower fully
Mixing, N, the N ＇-methylene-bisacrylamide adding 12.5mg makees cross-linking agent, continuously stirred, is passed through nitrogen, is slowly heated, poly-
Close after reaction starts, stop stirring, between 80-100 DEG C, be incubated 2h, drying, pulverize and i.e. obtain nitrogenous and potassium High hydrophilous resin, this
Under the conditions of synthesis product high water absorption in the deionized water of 5000 times be 770g/g.
Embodiment 5: weigh under 5g potato starch stirs with 40mL deionized water and mix homogeneously, 70 DEG C and the lower addition of stirring
The hydrogen peroxide of the 30% of 0.8mL oxidation reaction 1.5h；Weigh 12.96g potassium hydroxide, and with 20mL deionized water dissolving hydrogen
Potassium oxide；Ice-water bath cool down under with in the potassium hydroxide solution of described preparation and 31.7mL(33.3g) acrylic acid, obtain third
Olefin(e) acid and potassium salt soln thereof.Weigh 6.67g acrylamide, with 20mL deionized water dissolving acrylamide, obtain acrylamide molten
Liquid.By under the acrylic acid after above-mentioned oxidised potato starch solution and neutralization and potassium salt soln and acrylamide solution stirring thereof
Being sufficiently mixed, N, the N ＇-methylene-bisacrylamide adding 7.5mg makees cross-linking agent, continuously stirred, is passed through nitrogen, is slowly heated,
After polyreaction starts, stop stirring, between 80-100 DEG C, be incubated 2h, drying, pulverize and i.e. obtain nitrogenous and potassium High hydrophilous resin,
Under the conditions of this, product high water absorption in the deionized water of 5000 times of synthesis is 700g/g.
Claims (2)
1., with potato starch for raw material one kettle way graft copolymerization synthesis containing potassium and the method for the High hydrophilous resin of nitrogen, it is characterised by
Its method and step be:
(1) potato starch is under agitation mixed homogeneously by the mass ratio of 1:8 with deionized water, add Rhizoma Solani tuber osi at 70 DEG C and form sediment
The hydrogen peroxide oxidation 0.5h of the 30% of opaque amount 0.1776 times；Weigh the potassium hydroxide of potato quality 2.592 times, use hydrogen-oxygen
Change the deionized water dissolving of potassium quality 1.54 times；Use in the potassium hydroxide solution of preparation under ice-water bath cools down and potato starch
The acrylic acid removing polymerization inhibitor of quality 6.67 times；Weigh the acrylamide of potato starch quality 1.334 times, with acrylamide
The deionized water dissolving acrylamide of quality 3 times；
(2) by above-mentioned oxidised potato starch solution with neutralize after acrylic acid and potassium salt soln and acrylamide solution fill
Dividing mixing, add N, the N ＇-methylene-bisacrylamide containing potato starch quality 0.25% and make cross-linking agent, stirring is allowed to equal
Even, it is passed through nitrogen, is slowly heated, after polyreaction starts, stop stirring, between 80-100 DEG C, be incubated 2h, drying, pulverizing are i.e.
Obtaining nitrogenous and potassium High hydrophilous resin, under the conditions of being somebody's turn to do, product high water absorption in the deionized water of 5000 times of synthesis is 950g/
g。
The most according to claim 1, each raw materials quality is than for potato starch: the hydrogen peroxide of 30%: acrylic acid: hydroxide
Potassium: acrylamide: N, N ＇-methylene-bisacrylamide: total Water=1:0.1776:6.67:2.592:1.334:0.0025:
16；Wherein total Water is the dispersion water consumption of potato starch, dissolved hydrogen potassium oxide water consumption and dissolves acrylamide water consumption
Summation.
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| CN201610481266.1A CN106046261A (en) | 2016-06-28 | 2016-06-28 | Method for synthesizing super absorbent resin containing potassium and nitrogen through one-pot graft copolymerization with potato starch as raw material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021165842A1 (en) * | 2020-02-20 | 2021-08-26 | Upl Limited | A process for preparation of superabsorbent polymer |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| PL217380B1 (en) * | 2011-02-07 | 2014-07-31 | Univ West Pomeranian Szczecin Tech | Starch graft copolymer with high degree of solubility in water and method of obtaining of the starch hydrophilic graft copolymer with high degree of solubility in water |
| CN104163888A (en) * | 2014-07-08 | 2014-11-26 | 内蒙古大学 | Method for preparing super absorbent resin by grafting and copolymerizing potato starch oxidized through hydrogen peroxide |
| CN104177545A (en) * | 2014-07-08 | 2014-12-03 | 内蒙古大学 | Method for preparing super absorbent resin through graft polymerization of hydrogen peroxide-oxidized potato starch |
-
2016
- 2016-06-28 CN CN201610481266.1A patent/CN106046261A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| PL217380B1 (en) * | 2011-02-07 | 2014-07-31 | Univ West Pomeranian Szczecin Tech | Starch graft copolymer with high degree of solubility in water and method of obtaining of the starch hydrophilic graft copolymer with high degree of solubility in water |
| CN104163888A (en) * | 2014-07-08 | 2014-11-26 | 内蒙古大学 | Method for preparing super absorbent resin by grafting and copolymerizing potato starch oxidized through hydrogen peroxide |
| CN104177545A (en) * | 2014-07-08 | 2014-12-03 | 内蒙古大学 | Method for preparing super absorbent resin through graft polymerization of hydrogen peroxide-oxidized potato starch |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021165842A1 (en) * | 2020-02-20 | 2021-08-26 | Upl Limited | A process for preparation of superabsorbent polymer |
| US20230074309A1 (en) * | 2020-02-20 | 2023-03-09 | Upl Limited | A process for preparation of superabsorbent polymer |
| US11958925B2 (en) * | 2020-02-20 | 2024-04-16 | Upl Ltd | Process for preparation of superabsorbent polymer |
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Application publication date: 20161026 |