CN106117441A - The method being raw material one kettle way glycerol polymerization synthesizing super absorbent resin with potato starch - Google Patents
The method being raw material one kettle way glycerol polymerization synthesizing super absorbent resin with potato starch Download PDFInfo
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- CN106117441A CN106117441A CN201610480649.7A CN201610480649A CN106117441A CN 106117441 A CN106117441 A CN 106117441A CN 201610480649 A CN201610480649 A CN 201610480649A CN 106117441 A CN106117441 A CN 106117441A
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- potato starch
- acrylic acid
- water
- stirring
- high hydrophilous
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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 kind of method being raw material one kettle way glycerol polymerization synthesizing super absorbent resin with potato starch; its be mainly characterized by after hydrogen peroxide oxidation potato starch with remove the acrylic acid of polymerization inhibitor and sodium salt thereof in the presence of cross-linking agent, nitrogen protection and heating in water bath one pot process High hydrophilous resin, product in the deionized water of 5000 times high water absorption up to 2200g/g.The preparation of High hydrophilous resin of the present invention has the advantage that hydrogen peroxide oxidation potato starch needs not move through traditional separating oxidised potato starch and wash; mixture after oxidation self can serve as initiator; need not additionally add initiator; High hydrophilous resin synthesized by Tong Shi has higher water absorption; so the process of synthesizing super absorbent resin of the present invention is simple; low cost, properties of product are excellent, it is easier to large-scale production and the popularization of product.
Description
Technical field
The present invention relates to a kind of for fields such as agricultural gardening, physiological hygiene, daily-use chemical industry, building trade, environmental improvements
The preparation method of functional high molecule material High hydrophilous resin, particularly relate to potato starch, hydrogen peroxide, acrylic acid and
Sodium hydroxide is the method that primary raw material one kettle way prepares High hydrophilous resin.
Background technology
Super absorbent resin is to contain polar group in molecule and have the functional polymer material of three-dimensional crosslinked network structure
Material, it can absorb the water of own wt hundred times to thousand of times.High hydrophilous resin is with its water absorption, water-retaining property, sting to external world
Swash responsiveness and the complexing power of heavy metal ion and be used widely, as physiological hygiene articles for use, defend and control sand, city
City's greening and the field such as agricultural and gardening have a wide range of applications.
The at present research about High hydrophilous resin gets more and more, but water absorbent rate is the highest, complex technical process and high in cost of production
Problem always makes the problem that researcher is puzzled, and the polymerization of High hydrophilous resin needs the initiation of initiator, and initiator mainly has certainly
By base (such as azo and persulfate etc.) initiator and redox initiator two class, but the shortcoming of this two classes initiator is
Foreign ion can be introduced, eventually affect the water absorption of High hydrophilous resin.Therefore, these problems of the most just right solution are
Current research emphasis.
The application uses hydrogen peroxide oxidation potato starch and acrylic acid and the sodium salt one pot thereof removing polymerization inhibitor first
Method synthesizing super absorbent resin, traditional method is first to use hydrogen peroxide oxidation potato starch, through separating, washing, the step such as drying
Suddenly prepare oxidised potato starch, then be polymerized with monomer with oxidised potato starch for raw material and prepare High hydrophilous resin, this Shen
Eliminate the most well oxidised potato starch separation, wash, the step such as drying, and be not required to when synthesizing super absorbent resin
Initiator to be added, the product simultaneously prepared has higher water absorption, and high water absorption is up to 2200g/g.Therefore, the present invention
Technique is simple, synthesizes low cost, practical, has good application and popularization value.
Summary of the invention
The invention provides a kind of technique is simple, synthesis low cost, water absorbing capacity are strong super absorbent resin fat prod and system thereof
Preparation Method.
Its method and step are as follows:
(1) potato starch is under agitation mixed homogeneously by the mass ratio of 1:7 with deionized water, at 70 DEG C, add Rhizoma Solani tuber osi
The hydrogen peroxide of the 30% of starch quality 0.222 times, oxidation reaction 1h at this temperature and stirring；Weigh potato quality 1.67
Sodium hydroxide again, with the deionized water dissolving sodium hydroxide of sodium hydroxide quality 3 times；Then use under ice-water bath cooling and stirring
Prepare sodium hydroxide solution in and potato starch quality 6 times remove polymerization inhibitor acrylic acid, obtain acrylic acid and sodium thereof
Saline solution.
(2) by the potato starch solution after above-mentioned oxidation with neutralize after acrylic acid and sodium salt solution under agitation fill
Dividing mixing, N, the N ＇-methylene-bisacrylamide adding potato starch quality 0.2% makees cross-linking agent, and stirring is allowed to uniform, logical
Enter nitrogen, be slowly heated, make temperature of reaction system be stepped up, after beginning to be polymerized, stop stirring, be incubated between 80-100 DEG C
2h, drying, pulverizes and i.e. obtains High hydrophilous resin.The product obtained by experiment high water absorption in the deionized water of 5000 times
Reach 2200g/g.
Advantages of the present invention:
(1) present invention uses potato starch to be that raw material one kettle way prepares High hydrophilous resin, and the method technique is simple, be prone to behaviour
Make.
(2) without adding initiator i.e. polymerizable, impurity, low cost will not be introduced.
(3) hydrogen peroxide catabolite is water, pollution-free, simultaneously obtained by product there is excellent performance.
Accompanying drawing and subordinate list explanation
Fig. 1 is the process chart preparing High hydrophilous resin with potato starch one kettle way
Fig. 2 is the consumption of the 30% hydrogen peroxide influence curve to High hydrophilous resin water absorption
Fig. 3 is the oxidizing temperature of the potato starch influence curve to High hydrophilous resin water absorption
Fig. 4 is the oxidization time of the potato starch influence curve to High hydrophilous resin water absorption
Fig. 5 is potato starch and the acrylic acid mass ratio influence curve to High hydrophilous resin water absorption
Fig. 6 is acrylic acid degree of neutralization influence curve to High hydrophilous resin water absorption
Fig. 7 is the consumption of the cross-linking agent influence curve to High hydrophilous resin water absorption
Fig. 8 is the total Water of the reaction system influence curve to High hydrophilous resin water absorption
Fig. 9 is factor and the water-glass of High hydrophilous resin orthogonal experiment
Figure 10 is High hydrophilous resin orthogonal experiment data result table.
Detailed description of the invention
Embodiment 1: weigh under 5g potato starch stirs with 35mL deionized water and mix homogeneously, add at 70 DEG C
The hydrogen peroxide of 1mL30%, and oxidation reaction 1h at this temperature and stirring；Measure 28.6mL (30g) and remove the propylene of polymerization inhibitor
Acid, weighs 8.33g sodium hydroxide and is dissolved in 25mL deionized water, cools down at ice-water bath with above-mentioned prepared sodium hydroxide solution
Lower neutralization acrylic acid, obtains acrylic acid and sodium salt solution thereof；Acrylic acid after neutralizing and sodium salt solution and oxidised potato
It is sufficiently mixed under starch solution stirring uniformly, adds N, the N ＇-methylene-bisacrylamide of 7.5mg, at stirring, N2Under protection,
Being slowly heated and make system temperature be stepped up, reaction to be polymerized stops stirring after starting, and is incubated 2h, product warp between 80-100 DEG C
Dry, pulverize and i.e. obtain product, the High hydrophilous resin water absorption obtained by the present embodiment be 2200g/g.
Embodiment 2: weigh 5g potato starch and under agitation mix homogeneously with 40mL deionized water, adds at 70 DEG C
The hydrogen peroxide of 1mL30%, and oxidation reaction 1h at this temperature and stirring；Measure 28.6mL (30g) and remove the propylene of polymerization inhibitor
Acid, weighs 8.33g sodium hydroxide and is dissolved in 20mL deionized water, with above-mentioned prepared sodium hydroxide solution under ice-water bath cools down
Neutralize acrylic acid, obtain acrylic acid and sodium salt solution thereof；Acrylic acid and sodium salt solution thereof after neutralizing form sediment with oxidised potato
It is sufficiently mixed uniformly under powder solution stirring, adds 10mg N, N ＇-methylene-bisacrylamide, at stirring, N2Under protection, slowly
Heating makes system temperature be stepped up, and after reaction to be polymerized starts, stops stirring, is incubated 2h, drying, powder between 80-100 DEG C
Broken i.e. obtain product.It is 1850g/g by the High hydrophilous resin water absorption obtained by the present embodiment.
Embodiment 3: weigh 5g potato starch and under agitation mix homogeneously with 40mL deionized water, adds at 70 DEG C
The hydrogen peroxide of 1mL30%, oxidation reaction 1h at this temperature and stirring；Measure 28.6mL (30g) and remove the propylene of polymerization inhibitor
Acid, weighs 6.67g sodium hydroxide and is dissolved in 20mL deionized water, with above-mentioned prepared sodium hydroxide solution under ice-water bath cools down
Neutralize acrylic acid, obtain acrylic acid and sodium salt solution thereof；Acrylic acid and sodium salt solution thereof after neutralizing form sediment with oxidised potato
It is sufficiently mixed uniformly under powder solution stirring, adds 15mg N, N ＇-methylene-bisacrylamide, at stirring, N2Under protection, slowly
Heating makes system temperature be stepped up, and after reaction to be polymerized starts, stops stirring, is incubated 2h, drying, powder between 80-100 DEG C
Broken i.e. obtain product.It is 2165g/g by the High hydrophilous resin water absorption obtained by the present embodiment.
Embodiment 4: weigh under 5g potato starch stirs with 40mL deionized water and mix homogeneously, add at 70 DEG C
The hydrogen peroxide of 1mL30%, oxidation reaction 1h at this temperature and stirring；Measure 28.6mL (30g) and remove the propylene of polymerization inhibitor
Acid, weighs 11.67g sodium hydroxide and is dissolved in 25mL deionized water, cools down at ice-water bath with above-mentioned prepared sodium hydroxide solution
Lower neutralization acrylic acid, obtains acrylic acid and sodium salt solution thereof；Acrylic acid after neutralizing and sodium salt solution and oxidised potato
It is sufficiently mixed under starch solution stirring uniformly, adds 15mg N, N ＇-methylene-bisacrylamide, at stirring, N2Under protection, slow
Slow heating makes system temperature be stepped up, and after reaction to be polymerized starts, stops stirring, insulation 2h between 80-100 DEG C, drying,
Pulverize and i.e. obtain product.It is 2000g/g by the High hydrophilous resin water absorption obtained by the present embodiment.
Embodiment 5: weigh under 5g potato starch stirs with 25mL deionized water and mix homogeneously, add at 50 DEG C
The hydrogen peroxide of 1mL30%, and oxidation reaction 1h at this temperature and stirring；Measure 23.8mL (25g) and remove the propylene of polymerization inhibitor
Acid, weighs 6.94g sodium hydroxide and is dissolved in 25mL deionized water, with above-mentioned prepared sodium hydroxide solution under ice-water bath cools down
Neutralize acrylic acid, obtain acrylic acid and sodium salt solution thereof；Acrylic acid and sodium salt solution thereof after neutralizing form sediment with oxidised potato
It is sufficiently mixed uniformly under powder solution stirring, adds 15mg N, N ＇-methylene-bisacrylamide, at stirring, N2Under protection, slowly
Heating makes system temperature be stepped up, and after reaction to be polymerized starts, stops stirring, is incubated 2h, drying, powder between 80-100 DEG C
Broken i.e. obtain product.It is 1400g/g by the High hydrophilous resin water absorption obtained by the present embodiment.
Embodiment 6: weigh 5g potato starch and under agitation mix homogeneously with 50mL deionized water, adds at 70 DEG C
The hydrogen peroxide of 1mL30%, oxidation reaction 1h at this temperature and stirring；Measure 28.6mL (30g) and remove the propylene of polymerization inhibitor
Acid, weighs 8.33g sodium hydroxide and is dissolved in 20mL deionized water, with the sodium hydroxide solution of above-mentioned preparation under ice-water bath cools down
Neutralize acrylic acid, obtain acrylic acid and sodium salt solution thereof；Acrylic acid and sodium salt solution thereof after neutralizing form sediment with oxidised potato
Powder solution is under agitation sufficiently mixed uniformly, adds 15mg N, N ＇-methylene-bisacrylamide, at stirring, N2Under protection, slow
Slow heating makes system temperature be stepped up, and after reaction to be polymerized starts, stops stirring, insulation 2h between 80-100 DEG C, drying,
Pulverize and i.e. obtain product.It is 1500g/g by the High hydrophilous resin water absorption obtained by the present embodiment.
Claims (2)
1., with potato starch for the method for raw material one kettle way glycerol polymerization synthesizing super absorbent resin, it is characterised by its method and step
Suddenly it is:
(1) mix homogeneously under potato starch being stirred by the mass ratio of 1:7 with deionized water, at 70 DEG C, add Rhizoma Solani tuber osi form sediment
The hydrogen peroxide of the 30% of opaque amount 0.222, oxidation reaction 1h at this temperature and stirring；Weigh potato quality 1.67 times
Sodium hydroxide, with the deionized water dissolving of sodium hydroxide quality 3 times；With the hydrogen-oxygen of preparation under ice-water bath cooling, stirring condition
Change in sodium solution and the acrylic acid removing polymerization inhibitor of potato starch quality 6 times, obtain acrylic acid and sodium salt solution thereof；
(2) by the potato starch solution after above-mentioned oxidation with neutralize after acrylic acid and sodium salt solution the most mixed
Closing, add N, the N ＇-methylene-bisacrylamide containing potato starch quality 0.2% and make cross-linking agent, stirring is allowed to uniform, logical
Enter nitrogen, be slowly heated, make temperature of reaction system be stepped up, after reaction to be polymerized starts, stop stirring, 80-100 DEG C it
Between be incubated 2h, drying, pulverize and i.e. obtain High hydrophilous resin, product high water absorption in the deionized water of 5000 times reaches
2200g/g。
The most according to claim 1, each raw materials quality is than for potato starch: the hydrogen peroxide of 30%: acrylic acid: hydroxide
Sodium: N, N ＇-methylene-bisacrylamide: total Water=1:0.222:6: 1.67: 0.002:12；Wherein total Water is dispersion
The water consumption of potato starch and the water consumption sum of dissolved hydrogen sodium oxide.
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| CN201610480649.7A CN106117441A (en) | 2016-06-28 | 2016-06-28 | The method being raw material one kettle way glycerol polymerization synthesizing super absorbent resin with potato starch |
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| CN201610480649.7A CN106117441A (en) | 2016-06-28 | 2016-06-28 | The method being raw material one kettle way glycerol polymerization synthesizing super absorbent resin with potato starch |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1640901A (en) * | 2004-01-09 | 2005-07-20 | 中国科学院沈阳应用生态研究所 | Method for preparing resin type water-retaining preparation |
| CN101974126A (en) * | 2010-10-09 | 2011-02-16 | 内蒙古大学 | Method for synthesizing low-cost and super-absorbent resin from potato starch serving as raw material |
| 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 CN201610480649.7A patent/CN106117441A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1640901A (en) * | 2004-01-09 | 2005-07-20 | 中国科学院沈阳应用生态研究所 | Method for preparing resin type water-retaining preparation |
| CN101974126A (en) * | 2010-10-09 | 2011-02-16 | 内蒙古大学 | Method for synthesizing low-cost and super-absorbent resin from potato starch serving as raw material |
| 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 |
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Application publication date: 20161116 |