CN102344532A - Method for synthesizing super absorbent resin by using invasive plant - Google Patents
Method for synthesizing super absorbent resin by using invasive plant Download PDFInfo
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- CN102344532A CN102344532A CN2011102052473A CN201110205247A CN102344532A CN 102344532 A CN102344532 A CN 102344532A CN 2011102052473 A CN2011102052473 A CN 2011102052473A CN 201110205247 A CN201110205247 A CN 201110205247A CN 102344532 A CN102344532 A CN 102344532A
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Abstract
The invention provides a method for synthesizing super absorbent resin by using an invasive plant. The method is characterized by comprising the following specific steps of: crushing a straw of the invasive plant; adding the crushed straw in an alkaline solution; heating, washing and drying; adding the dried mixture in an acid solution; heating, washing and drying; further crushing the mixture by using a crusher to obtain cellulose; sequentially adding acrylic acid solution, initiator solution and mixed solution of acrylamide and a cross-linking agent in the obtained cellulose; uniformly stirring; heating in a water bath to be 65-95DEG C; carrying out polymerization reaction and stopping stirring until a system is gelatinous; taking out the obtained gelatin; washing with ethanol or acetone; and suction filtering and vacuum drying to obtain the super absorbent resin. According to the method disclosed by the invention, the invasive plant is used a plant raw material, and thus the production cost is reduced and the environment can be protected.
Description
Technical field
The present invention relates to a kind of method of utilizing the instruction plant synthesizing high-hydroscopicity resin, belong to the polymer water uptake expansion resin technical field.
Background technology
Super absorbent resin is the novel high polymer material that contains the strong hydrophilicity group that begins to grow up from the sixties in 20th century.It is as a kind of novel functional high molecule material; Since being born, received widely always and paying close attention to; Its strongly hydrophilic group and degree of crosslinking; Can absorb the water of hundreds of times of himself quality even thousands of times and swelling is gel through hydration; Water can not separated out under certain pressure, can recover its water absorbing properties after the jello drying.
Common super absorbent resin has three types, i.e. starch system, synthetic system and cellulose-based.Publication number is the preparation method that the Chinese patent of CN 101864036 A discloses a kind of Super Absorbent Resin from Cellulose.This method is in the superpower super absorbent resin process of cellulose modified synthetic; Need the preparation carboxymethyl cellulose, divide etherificate and crosslinked two steps, and cellulosic etherificate need be used Mono Chloro Acetic Acid reagent; This reagent is a kind of toxic reagent, when producing, can produce certain influence to human body and environment.Need activate 0.5 ~ 2h in the polymeric reactions step, add initiator (NH
4)
2S
2O
8Cause 0.5 ~ 2h, the adding degree of neutralization is prepolymer heating in water bath for reaction 1 ~ 5h of 50% ~ 80%, adds linking agent and continues reaction 1-3h, obtains super absorbent resin.This synthesis step is comparatively loaded down with trivial details, and cycle production time is longer, unfavorable scale production, and unreacted toxic reagent completely can pollute environment.
Summary of the invention
Technical problem to be solved by this invention provides a kind of method of utilizing depleted exotic invasive phytosynthesis super absorbent resin; It can be through lower cost, simple steps and short production cycle synthesizing high-hydroscopicity resin, and the super absorbent resin water-retaining capacity of producing strong, nontoxic, be easy to environment degradable.
In order to achieve the above object, the invention provides a kind of method of utilizing the instruction plant synthesizing high-hydroscopicity resin, it is characterized in that concrete steps are:
The first step: with the instruction plant crushed stalk, it is joined in the alkaline solution, heat treated, washing, oven dry joins it in acid solution again, heat treated, washing, oven dry obtains Mierocrystalline cellulose with further pulverizing of pulverizer;
Second step: prepare acrylic acid solution, initiator solution, acrylamide soln and cross-linking agent solution respectively, regulate pH value to 6 ~ 8 of acrylic acid solution, cross-linking agent solution is joined the mixing solutions that obtains acrylamide and linking agent in the acrylamide soln;
The 3rd step: in the Mierocrystalline cellulose of the first step gained, add acrylic acid solution, initiator solution and the acrylamide of the second step gained and the mixing solutions of linking agent successively; Stir; Heating in water bath is warming up to 65 ~ 95 ℃; Polyreaction stops to stir (this process is about 9 ~ 20 minutes) when system is glue, takes out the gel of gained; With ethanol or washing with acetone; Suction filtration, vacuum-drying promptly obtains super absorbent resin.
Preferably, the instruction plant in the said the first step is a composite family Herba Solidaginis platymiscium Herba Solidaginis.
Preferably, the length after instruction plant is pulverized in the said the first step is 1 ~ 5mm.
Preferably, the alkaline solution in the said the first step is that mass percent concentration is 3% ~ 15% sodium hydroxide or potassium hydroxide solution, and the temperature of heating is 130 ~ 170 ℃, and the treatment time is 5-30 minute, and bake out temperature is controlled at 50 ~ 90 ℃.
Preferably, the acid solution in the said the first step is 0.5 ~ 1.5mol/L salpeter solution, and the temperature of heating is 80 ~ 120 ℃, and the treatment time is 20-40 minute.
Preferably, the initiator in said second step is to be heated to resolve into the compound of free radical easily, is preferably the persulphate system, like Potassium Persulphate or ammonium persulphate.
Preferably, the initiator in said second step and the cellulosic weight ratio of the first step gained are 0.002 ~ 0.5:1.
Preferably, the linking agent in said second step is a N,N methylene bis acrylamide, and the cellulosic weight ratio of itself and the first step gained is 0.001 ~ 0.03:1.
Preferably, the acrylamide in said second step and the cellulosic weight ratio of the first step gained are 1 ~ 12:1.
Preferably, the vinylformic acid in said second step and the cellulosic ratio of the first step gained are 2 ~ 15ml:1g.
Advantage of the present invention is:
1, the present invention as plant material, can not only reduce production costs instruction plant, and can protect environment;
2, the present invention is through simple steps and short production cycle synthesizing high-hydroscopicity resin, and the super absorbent resin water-retaining capacity of producing strong, nontoxic, be easy to environment degradable.
Description of drawings
Fig. 1 is the infrared spectra comparison diagram before and after the grafting of instruction plant starting material.
Embodiment
Specify the present invention below in conjunction with embodiment.Used N among the embodiment 1-3; The N-methylene-bisacrylamide is available from Chemical Reagent Co., Ltd., Sinopharm Group; Potassium Persulphate is available from Shanghai fine chemistry industry Science and Technology Ltd., and acrylamide is available from Shanghai fine chemistry industry Materials Research Laboratories, and vinylformic acid (AA) is available from Chemical Reagent Co., Ltd., Sinopharm Group.Among the embodiment 1-3 used instruction plant be composite family Herba Solidaginis platymiscium Herba Solidaginis (
Solidago CanadensisL.).
Embodiment 1
The solidago canadesis straw is crushed to 3 ~ 4mm, and oven dry adds mass percent concentration and is 14% sodium hydroxide solution in 170 ℃ of following oil bath boilings 5 minutes, and its water is washed till pH=7, puts into 50 ℃ of oven dry down of vacuum drying oven.The nitric acid that adds 0.5mol/L was then handled 40 minutes down at 80 ℃, and the soda cellulose water that obtains is washed till pH=7, and oven dry is for use.
The solution preparation is respectively: get 4ml vinylformic acid and be dissolved in the 12ml distilled water, the sodium hydroxide with 25% is neutralized to pH=6; The 0.86g Potassium Persulphate is dissolved in the 6.4ml distilled water; The 24g acrylamide is dissolved in the 22ml distilled water; 0.017g linking agent N,N methylene bis acrylamide is dissolved in the 6.4ml distilled water; Again the cross-linking agent solution for preparing is added in the middle of the acrylamide, stir.
Get the 2g soda cellulose in reaction vessel; Add vinylformic acid neutralization solution, potassium persulfate solution, acrylamide and the linking agent mixed solution that configures successively,, when system is glue, stop to stir in 65 ℃ of following heating in water bath polyreactions; Take out gel; Use washing with alcohol,, product is dried in 60 ℃ vacuum drying oven with circulation ability of swimming vacuum pump suction filtration; Pulverize; Can obtain super absorbent resin, record its suction distilled water multiplying power and reach 579g/g, inhale the salt solution multiplying power and reach 83g/g.
As shown in Figure 1, be the infrared spectra comparison diagram before and after the grafting of instruction plant starting material.The a line is the infrared spectra curve of unreacted fiber, and the b line is the infrared spectra curve of the water-absorbing resin of reaction generation.From figure, can find out, at 2925cm
-1The C-H stretching vibration that the place occurs, at 1648cm
-1C=H stretching vibration, 1507 cm that the place occurs
-1The C=C skeletal vibration that the place occurs and at 1379 cm
-1With 668 cm
-1For out-of-plane bending etc. is located before and after the peak position all less than change, and 1172 cm in the b line
-1The place occurred saturated ester C-C (=O)-the O bands of a spectrum, illustrate that esterification has taken place for solidago canadesis and vinylformic acid.At 1049 cm
-1It is flexible that ether R-O has appearred in the place, illustrates that the O-H key of solidago canadesis ruptures, and produced ehter bond, and the generation of graft reaction has been described.
Embodiment 2
The solidago canadesis straw is crushed to 3 ~ 4mm, and oven dry adds mass percent concentration and is 11% sodium hydroxide solution in 130 ℃ of following oil bath boilings 30 minutes, and its water is washed till pH=7, puts into 90 ℃ of oven dry down of vacuum drying oven.Combine the nitric acid of 1.5mol/L to handle 20 minutes down at 120 ℃ then, the soda cellulose water that obtains is washed till pH=7, and oven dry is for use.
The solution preparation is respectively: get 16.5ml vinylformic acid and be dissolved in the 12ml distilled water, the sodium hydroxide with 25% is neutralized to pH=7; The 0.1g Potassium Persulphate is dissolved in the 6.4ml distilled water; The 2g acrylamide is dissolved in the 22ml distilled water; 0.06g linking agent N,N methylene bis acrylamide is dissolved in the 6.4ml distilled water; Again the cross-linking agent solution for preparing is added in the middle of the acrylamide, stir.
Get the 2g soda cellulose in reaction vessel; Add vinylformic acid neutralization solution, potassium persulfate solution, acrylamide and the linking agent mixed solution that configures successively,, when system is glue, stop to stir in 85 ℃ of following heating in water bath polyreactions; Take out gel; Use washing with alcohol,, product is dried in 60 ℃ vacuum drying oven with circulation ability of swimming vacuum pump suction filtration; Pulverize; Can obtain super absorbent resin, record its suction distilled water multiplying power and reach 494g/g, inhale the salt solution multiplying power and reach 74g/g.
Embodiment 3
The solidago canadesis straw is crushed to 3 ~ 4mm, and oven dry adds mass percent concentration and is 3% sodium hydroxide solution in 150 ℃ of following oil bath boilings 30 minutes, and its water is washed till pH=7, puts into 60 ℃ of oven dry down of vacuum drying oven.Combine the nitric acid of 1mol/L to handle 30 minutes down at 100 ℃ then, the soda cellulose water that obtains is washed till pH=7, and oven dry is for use.
The solution preparation is respectively: get 30ml vinylformic acid and be dissolved in the 12ml distilled water, the sodium hydroxide with 25% is neutralized to pH=8; The 0.96g Potassium Persulphate is dissolved in the 6.4ml distilled water; The 24g acrylamide is dissolved in the 22ml distilled water; 0.008g linking agent N,N methylene bis acrylamide is dissolved in the 6.4ml distilled water; Again the cross-linking agent solution for preparing is added in the middle of the acrylamide, stir.
Get the 2g soda cellulose in reaction vessel; Add vinylformic acid neutralization solution, potassium persulfate solution, acrylamide and the linking agent mixed solution that configures successively,, when system is glue, stop to stir in 95 ℃ of following heating in water bath polyreactions; Take out gel; Use washing with alcohol,, product is dried in 60 ℃ vacuum drying oven with circulation ability of swimming vacuum pump suction filtration; Pulverize; Can obtain super absorbent resin, record its suction distilled water water multiplying power and reach 473g/g, inhale the salt solution multiplying power and reach 77g/g.
Claims (10)
1. a method of utilizing the instruction plant synthesizing high-hydroscopicity resin is characterized in that, concrete steps are:
The first step: with the instruction plant crushed stalk, it is joined in the alkaline solution, heat treated, washing, oven dry joins it in acid solution again, heat treated, washing, oven dry obtains Mierocrystalline cellulose with further pulverizing of pulverizer;
Second step: prepare acrylic acid solution, initiator solution, acrylamide soln and cross-linking agent solution respectively, regulate pH value to 6 ~ 8 of acrylic acid solution, cross-linking agent solution is joined the mixing solutions that obtains acrylamide and linking agent in the acrylamide soln;
The 3rd step: in the Mierocrystalline cellulose of the first step gained, add acrylic acid solution, initiator solution and the acrylamide of the second step gained and the mixing solutions of linking agent successively; Stir; Heating in water bath is warming up to 65 ~ 95 ℃; Polyreaction stops to stir when system is glue, takes out the gel of gained; With ethanol or washing with acetone; Suction filtration, vacuum-drying promptly obtains super absorbent resin.
2. the method for utilizing the instruction plant synthesizing high-hydroscopicity resin as claimed in claim 1 is characterized in that, the instruction plant in the said the first step is a composite family Herba Solidaginis platymiscium Herba Solidaginis.
3. the method for utilizing the instruction plant synthesizing high-hydroscopicity resin as claimed in claim 1 is characterized in that, the length after instruction plant is pulverized in the said the first step is 1 ~ 5mm.
4. the method for utilizing the instruction plant synthesizing high-hydroscopicity resin as claimed in claim 1; It is characterized in that; Alkaline solution in the said the first step is that mass percent concentration is 3% ~ 15% sodium hydroxide or potassium hydroxide solution; The temperature of heating is 130 ~ 170 ℃; Treatment time is 5-30 minute, and bake out temperature is controlled at 50 ~ 90 ℃.
5. the method for utilizing the instruction plant synthesizing high-hydroscopicity resin as claimed in claim 1 is characterized in that, the acid solution in the said the first step is 0.5 ~ 1.5mol/L salpeter solution, and the temperature of heating is 80 ~ 120 ℃, and the treatment time is 20-40 minute.
6. the method for utilizing the instruction plant synthesizing high-hydroscopicity resin as claimed in claim 1 is characterized in that, the initiator in said second step is Potassium Persulphate or ammonium persulphate.
7. the method for utilizing the instruction plant synthesizing high-hydroscopicity resin as claimed in claim 1 is characterized in that, the initiator in said second step and the cellulosic weight ratio of the first step gained are 0.002 ~ 0.5:1.
8. the method for utilizing the instruction plant synthesizing high-hydroscopicity resin as claimed in claim 1 is characterized in that, the linking agent in said second step is a N,N methylene bis acrylamide, and the cellulosic weight ratio of itself and the first step gained is 0.001 ~ 0.03:1.
9. the method for utilizing the instruction plant synthesizing high-hydroscopicity resin as claimed in claim 1 is characterized in that, the acrylamide in described second step and the cellulosic weight ratio of the first step gained are 1 ~ 12:1.
10. the method for utilizing the instruction plant synthesizing high-hydroscopicity resin as claimed in claim 1 is characterized in that, the vinylformic acid in said second step and the cellulosic ratio of the first step gained are 2 ~ 15ml:1g.
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CN102675563A (en) * | 2012-05-17 | 2012-09-19 | 昆明理工大学 | Preparation method of water-absorbable material by crofton weed |
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CN103145921A (en) * | 2013-03-28 | 2013-06-12 | 东华大学 | Preparation method of high oil-absorption material based on invasive plant |
CN103254361A (en) * | 2013-06-07 | 2013-08-21 | 王永利 | Preparation method of straw-based water-retaining agent |
CN103524681A (en) * | 2012-07-03 | 2014-01-22 | 中国科学院兰州化学物理研究所 | Kapok fiber composite super absorbent resin as well as preparation method thereof |
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Application publication date: 20120208 |