CN104072672B - Method using carboxymethyl manioc waste as Material synthesis high hydroscopic resin - Google Patents
Method using carboxymethyl manioc waste as Material synthesis high hydroscopic resin Download PDFInfo
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- CN104072672B CN104072672B CN201410319564.1A CN201410319564A CN104072672B CN 104072672 B CN104072672 B CN 104072672B CN 201410319564 A CN201410319564 A CN 201410319564A CN 104072672 B CN104072672 B CN 104072672B
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- carboxymethyl
- manioc waste
- high hydroscopic
- hydroscopic resin
- acrylic acid
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Abstract
The invention discloses the method using carboxymethyl manioc waste as Material synthesis high hydroscopic resin; it is mainly characterized by under ice-water bath cooling first with sodium hydroxide and acrylic acid; then with N; N ＇ methylene-bisacrylamides are crosslinking agent, using potassium peroxydisulfate as initiator; the heating water bath under the protection of nitrogen, the acrylic acid and its sodium salt graft polymerization for making carboxymethyl manioc waste and part neutralization prepare high hydroscopic resin.Best product 1g highest water absorptions in 2500 times of deionized water reach 1773g/g.High hydroscopic resin of the present invention using carboxymethyl manioc waste as Material synthesis has the advantage that：Parent carboxymethyl manioc waste is soluble in water, need not be gelatinized; use low in raw material price, environmental protection and energy saving; so the high hydroscopic resin synthesis technique of the present invention is simple, easy to operate, cost is low, and properties of product are excellent, more preferably in large-scale production and the popularization of product.
Description
Technical field
The present invention relates to a kind of function for fields such as agricultural gardening, desertification treatment, building trade, environmental improvements is high
The preparation method of molecular material-high hydroscopic resin, refer in particular to using carboxymethyl manioc waste, acrylic acid, sodium hydroxide as primary raw material
A kind of new simple method for preparing of synthesizing super absorbent resin.
Background technology
Manioc waste is exactly that a kind of cassava caused main component after starch or alcohol is processed into is water, cell fragment, shallow lake
The accessory substance of powder, cellulose and a small amount of protein, usually as a kind of roughage letting animals feed.Fresh sweet potato slag carries strain crowd
It is more, it is not easy to store, transports, produces stench after putrid and deteriorated, cause environmental pollution;Cost is too high if drying, and increase enterprise bears
Load, makees burial processing usually as feed or as waste residue, does not like to eat as feed animals, burial can cause soil and groundwater
Pollution, while producing level is relatively low.Contain substantial amounts of cellulose in potato slag, there is very high value of exploiting and utilizing.By cassava
Carboxymethyl manioc waste, which is made, after alkalization, etherification reaction processing in slag to prepare high hydroscopic resin with it.
Super absorbent resin is three-dimensional netted functional high molecule material lightly crosslinked in a kind of new, structure.It
The water of own wt hundred times to thousands of times can be absorbed, it is good to light, heat, the stability of acid and alkali, also there is good biology drop
Solve performance.High hydroscopic resin with its water imbibition, water-retaining property, be used widely to performances such as the responsiveness of environmental stimuli,
Such as agricultural gardening, soil improvement, retain water and nutrients, hydrogel substrate, water-oil separating, encapsulant, nursery stock protection.
The content of the invention
The invention provides a kind of operating procedure is simple, water absorbing capacity is strong, low raw-material cost super absorbent resin fat prod
And preparation method thereof.
Its method and step are as follows：
（1）Carboxymethyl manioc waste and deionized water are pressed 1：8 mass ratio mixing；Weigh carboxymethyl manioc waste quality 4-12
Acrylic acid again, weighs the sodium hydroxide of 0.1113-0.3887 times of acrylic acid quality, is dissolved respectively with 27.5ml deionized water
The sodium hydroxide of above range；With in above-mentioned sodium hydroxide solution and acrylic acid under ice-water bath cooling；
（2）Above-mentioned carboxymethyl manioc waste and the mixed liquor of deionized water and the acrylic acid that is neutralized with sodium hydroxide part is molten
Liquid is well mixed in reaction vessel, is added the potassium persulfate solution containing carboxymethyl manioc waste quality 1%~5% and is made initiator,
The N containing carboxymethyl manioc waste quality 0.4%~1.2% is added, N ＇-methylene-bisacrylamide solution makees crosslinking agent, and stirring makes
It is well mixed, nitrogen is passed through, being stirred continuously slow heating is stepped up temperature of reaction system, when temperature rises to 70-80 DEG C
When stop stirring, continue heating and be incubated 2h when temperature reaches 90 DEG C after, taking-up product, drying, crush and produce high hydroscopic resin.
Best product 1g highest water absorptions in 2500 times of deionized water reach 1773g/g.
As described above, the alkali that the present invention neutralizes used in acrylic acid is sodium hydroxide, the concentration of the potassium persulfate solution of preparation
For 10mg/ml, N, the concentration of N ＇-methylene-bisacrylamide solution is 2mg/ml.
Advantages of the present invention：
（1）Carboxymethyl manioc waste is soluble in water, need not be gelatinized during prepared by high hydroscopic resin；
（2）Raw material manioc waste is cheap, cost-effective；
（3）Product water absorption is higher.
Brief description of the drawings：
Fig. 1 is the process chart of carboxymethyl manioc waste synthesizing super absorbent resin
Fig. 2 is the influence curve with degree of neutralization during acrylic acid to high hydroscopic resin water absorption in sodium hydroxide
Fig. 3 is influence curve of the initiator amount to high hydroscopic resin water absorption
Fig. 4 is influence curve of the dosage of crosslinking agent to high hydroscopic resin water absorption
Fig. 5 carboxymethyls manioc waste and acrylic acid with the influence curve for comparing high hydroscopic resin water absorption.
Embodiment
Embodiment 1：1.67g sodium hydroxides are weighed, are dissolved in 27.5ml deionized waters, weigh 15g acrylic acid, ice-water bath
Above-mentioned sodium hydroxide solution is added drop-wise into stirring in acrylic acid under cooling makes its neutralization（The degree of neutralization of acrylic acid is 20%）, weigh
2.5g carboxymethyls manioc waste is well mixed with 20ml deionized waters, by the acrylic acid after neutralization and its sodium salt and carboxymethyl manioc waste
Solution is well mixed, add 7.5ml concentration be 10mg/ml potassium persulfate solution, 10ml concentration be 2mg/ml N, N ＇-methylene
Base bisacrylamide solution, is passed through nitrogen, and being stirred continuously slow heating is stepped up temperature of reaction system, when temperature rises to
Stop stirring at 70-80 DEG C, continue heating and 2h is incubated after temperature reaches 90 DEG C, take out product, drying, crushing obtain high suction
Water-resin, water absorption of the high hydroscopic resin in 2500 times of deionized waters obtained by the present embodiment are 367g/g.
Embodiment 2：Synthesis condition is with embodiment 1, except that weighing 2.50g sodium hydroxides, is dissolved in 27.5ml and goes
In ionized water, 15g acrylic acid is weighed, above-mentioned sodium hydroxide solution is added drop-wise into stirring in acrylic acid under ice-water bath cooling makes wherein
With（The degree of neutralization of acrylic acid is 30%）, water absorption of the high hydroscopic resin in 2500 times of deionized waters is obtained by the present embodiment
681g/g。
Embodiment 3：Synthesis condition is with embodiment 1, except that weighing 3.33g sodium hydroxides, is dissolved in 27.5ml and goes
In ionized water, 15g acrylic acid is weighed, above-mentioned sodium hydroxide solution is added drop-wise into stirring in acrylic acid under ice-water bath cooling makes wherein
With（The degree of neutralization of acrylic acid is 40%）, water absorption of the high hydroscopic resin in 2500 times of deionized waters is obtained by the present embodiment
701g/g。
Embodiment 4：Synthesis condition is with embodiment 1, except that weighing 4.16g sodium hydroxides, is dissolved in 27.5ml and goes
In ionized water, 15g acrylic acid is weighed, above-mentioned sodium hydroxide solution is added drop-wise into stirring in acrylic acid under ice-water bath cooling makes wherein
With（The degree of neutralization of acrylic acid is 50%）, water absorption of the high hydroscopic resin in 2500 times of deionized waters is obtained by the present embodiment
732g/g。
Embodiment 5：Synthesis condition is with embodiment 1, except that weighing 5.00g sodium hydroxides, is dissolved in 27.5ml and goes
In ionized water, 15g acrylic acid is weighed, above-mentioned sodium hydroxide solution is added drop-wise into stirring in acrylic acid under ice-water bath cooling makes wherein
With（The degree of neutralization of acrylic acid is 60%）, water absorption of the high hydroscopic resin in 2500 times of deionized waters is obtained by the present embodiment
734g/g。
Embodiment 6：Synthesis condition is with embodiment 1, except that weighing 5.83g sodium hydroxides, is dissolved in 27.5ml and goes
In ionized water, 15g acrylic acid is weighed, above-mentioned sodium hydroxide solution is added drop-wise into stirring in acrylic acid under ice-water bath cooling makes wherein
With（The degree of neutralization of acrylic acid is 70%）, water absorption of the high hydroscopic resin in 2500 times of deionized waters is obtained by the present embodiment
798g/g。
Embodiment 7：5.00g sodium hydroxides are weighed, are dissolved in 27.5ml deionized waters, weigh 15g acrylic acid, ice-water bath
Above-mentioned sodium hydroxide solution is added drop-wise into stirring in acrylic acid under cooling makes its neutralization, weighs 2.5g carboxymethyls manioc waste and 20ml
Deionized water is well mixed, and the acrylic acid after neutralization and its sodium salt are well mixed with carboxymethyl manioc waste solution, adds 2.5ml
The N that potassium persulfate solution that concentration is 10mg/ml, 10ml concentration are 2mg/ml, N ＇-methylene-bisacrylamide solution, is passed through
Nitrogen, being stirred continuously slow heating is stepped up temperature of reaction system, stops stirring when temperature rises to 70-80 DEG C, continues
Heating is incubated 2h when temperature reaches 90 DEG C after, takes out product, drying, crushes and obtains high hydroscopic resin, obtained by the present embodiment
Water absorption of the high hydroscopic resin in 2500 times of deionized waters be 999g/g.
Embodiment 8：Synthesis condition is with embodiment 7, except that the potassium peroxydisulfate that 5ml concentration is 10mg/ml need to be added
Solution, water absorption of the high hydroscopic resin in 2500 times of deionized waters obtained by the present embodiment are 1282g/g.
Embodiment 9：Synthesis condition is with embodiment 7, except that the persulfuric acid that 7.5ml concentration is 10mg/ml need to be added
Potassium solution, water absorption of the high hydroscopic resin in 2500 times of deionized waters obtained by the present embodiment are 1364g/g.
Embodiment 10：Synthesis condition is with embodiment 7, except that the persulfuric acid that 10ml concentration is 10mg/ml need to be added
Potassium solution, water absorption of the high hydroscopic resin in 2500 times of deionized waters obtained by the present embodiment are 1435g/g.
Embodiment 11：Synthesis condition is with embodiment 7, except that the over cure that 12.5ml concentration is 10mg/ml need to be added
Sour potassium solution, water absorption of the high hydroscopic resin in 2500 times of deionized waters obtained by the present embodiment are 1135g/g.
Embodiment 12：Synthesis condition is with embodiment 7, except that the N, N ＇-methylene that 5ml concentration is 2mg/ml need to be added
Base bisacrylamide solution, water absorption of the high hydroscopic resin in 2500 times of deionized waters obtained by the present embodiment are 735g/g.
Embodiment 13：Synthesis condition is with embodiment 7, except that the N, N ＇-Asia that 7.5ml concentration is 2mg/ml need to be added
Bisacrylamide solution, water absorption of the high hydroscopic resin in 2500 times of deionized waters obtained by the present embodiment are 1090g/
g。
Embodiment 14：Synthesis condition is with embodiment 7, except that the N, N ＇-Asia that 10ml concentration is 2mg/ml need to be added
Bisacrylamide solution, water absorption of the high hydroscopic resin in 2500 times of deionized waters obtained by the present embodiment are 1773g/
g。
Embodiment 15：Synthesis condition is with embodiment 7, except that the N that 12.5ml concentration is 2mg/ml need to be added, N ＇-
Methylene-bisacrylamide solution, water absorption of the high hydroscopic resin in 2500 times of deionized waters is obtained by the present embodiment
1200g/g。
Embodiment 16：Synthesis condition is with embodiment 7, except that the N, N ＇-Asia that 15ml concentration is 2mg/ml need to be added
Bisacrylamide solution, water absorption of the high hydroscopic resin in 2500 times of deionized waters obtained by the present embodiment are 1101g/
g。
Claims (2)
1. using carboxymethyl manioc waste as the method for Material synthesis high hydroscopic resin, it is characterised by, its method and step are:
(1) carboxymethyl manioc waste and deionized water are pressed 1:8 mass ratio mixing;Weigh 4 ~ 12 times of carboxymethyl manioc waste quality
Acrylic acid, the sodium hydroxide of 0.1113 ~ 0.3887 times of acrylic acid quality is weighed, dissolved respectively with 27.5ml deionized water above-mentioned
The sodium hydroxide of scope;With in above-mentioned sodium hydroxide solution and acrylic acid under ice-water bath cooling;
(2) above-mentioned carboxymethyl manioc waste and the mixed liquor of deionized water are existed with the acrylic acid solution neutralized with sodium hydroxide part
It is well mixed in reaction bulb, adds the potassium persulfate solution containing carboxymethyl manioc waste quality 1 ~ 5% and make initiator, addition contains
The N of carboxymethyl manioc waste quality 0.4 ~ 1.2%, N '-methylene-bisacrylamide solution make crosslinking agent, and stirring is allowed to well mixed,
Nitrogen is passed through, being stirred continuously slow heating is stepped up temperature of reaction system, stops stirring when temperature rises to 70 ~ 80 DEG C,
Continue heating and be incubated 2h when temperature reaches 90 DEG C after, taking-up product, drying, crush and produce high hydroscopic resin.
2. the method according to claim 1 using carboxymethyl manioc waste as Material synthesis high hydroscopic resin, it is characterised in that
The concentration of the potassium persulfate solution of preparation is 10mg/ml, N, and the concentration of N '-methylene-bisacrylamide solution is 2mg/ml.
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| "以羧甲基纤维素合成含氮吸水剂及性质研究";塔娜等;《胶体与聚合物》;20060630;第24卷(第2期);24-25 * |
| "木薯渣综合利用研究";谢文伟等;《农牧产品开发》;19991025(第10期);10-11 * |
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