CN103554371A - Preparation method of starch-grafted polyacrylic acid super absorbent resin - Google Patents
Preparation method of starch-grafted polyacrylic acid super absorbent resin Download PDFInfo
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- CN103554371A CN103554371A CN201310578490.9A CN201310578490A CN103554371A CN 103554371 A CN103554371 A CN 103554371A CN 201310578490 A CN201310578490 A CN 201310578490A CN 103554371 A CN103554371 A CN 103554371A
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Abstract
The invention relates to a preparation method of starch-grafted polyacrylic acid super absorbent resin. The preparation method of the starch-grafted polyacrylic acid super absorbent resin is characterized by comprising the following step: by taking starch and acrylic acid as raw materials, carrying out starch dextrinization, neutralization through acrylic acid, starch grafting and subsequent treatment. The starch-grafted polyacrylic acid super absorbent resin prepared by the preparation method disclosed by the invention is low in production cost, high in water absorption and high in saline solution absorption, and meanwhile has good biodegradability.
Description
Technical field
The present invention relates to the preparation method of super absorbent resin, be specifically related to the preparation method of starch-grafted polymeric acrylic acid High hydrophilous resin.
Background technology
Absorbent resin is to have lightly crosslinked three-dimensional net structure, it is impelled between chemically crosslinked and molecular resin chain and to be mutually wound around physical crosslinking the two forms by linking agent, before water suction, macromolecular chain is drawn close together mutually, be cross-linked to each other and reticulate structure, thereby reach fastening degree on the whole, High hydrophilous resin can be regarded the ion network of polymer electrolyte composition and the construct of water as, its water-retaining capacity depends on the effect of repelling each other the ionic charge of polymer electrolyte in water the interaction of the stretching, extension causing and the prevention being caused by crosslinking structure and hydrogen bond expansion producing.
High hydrophilous resin is mainly used in fields such as agricultural, sanitary product, food, particularly sanitary product aspect increases day by day to the demand of High hydrophilous resin, greatly promoted the development of High hydrophilous resin, under this environment, polyacrylic super absorbent resin can be stablized and be paid close attention to widely because of its water-intake rate high-hydroscopicity, but because production cost is too high, cause application to be very limited, and polyacrylic super absorbent resin is pure organic-compound system, biological degradability is poor.
Summary of the invention
The present invention is intended to overcome the deficiency that prior art exists, and provides production cost low, and water-intake rate is high and suction salt solution multiplying power is high, the preparation method of the starch-grafted polymeric acrylic acid High hydrophilous resin that biological degradability is good.
The technical solution used in the present invention is as follows:
The preparation method of starch graft polyacrylic acid superabsorbent, is characterized in that it is raw material that the method be take starch and vinylformic acid, comprises following steps:
Described step
middle gelatinization point is 55 ℃-60 ℃.
Described step
middle degree of neutralization is 40%-60%.
Described step
middlely after pulverizing, sieving, obtain starch graft polyacrylic acid superabsorbent surface and carry out secondary crosslinking processing.
Compared with prior art, beneficial effect is in the present invention: obtained starch-grafted polymeric acrylic acid super absorbent resin production cost is low, and water-intake rate is high and suction salt solution multiplying power is high, possesses good biodegradability simultaneously.
Embodiment
Embodiment 1
40g starch is added in the there-necked flask with agitator, reflux exchanger and thermometer, drip 60g distilled water, cooling stir gelatinization 20min in 60 ℃ of waters bath with thermostatic control after, obtain pasted starch.In addition, the KOH solution 150g that preparation massfraction is 20% adds vinylformic acid 100g to make it neutralization in this solution, and degree of neutralization is 40%, is cooled to room temperature, obtains acrylate solution; The there-necked flask to 45 ℃ of pasted starch is housed with heating in water bath, add described acrylate solution, after stirring, the N of massfraction 0.4% successively, N '-methylene-bis acrylic acid amides solution 1g, the divinyl benzole soln 1g of massfraction 0.05%, continue to be warming up to 55 ℃, add the ammonium persulfate solution 5g of massfraction 0.1%, the ammonium sulfite solution 5g of massfraction 0.5%, stir 40min to reacting completely, obtain reaction product; Subsequently, reaction product is placed in to constant temperature oven, in 80 ℃ dry, obtain after crushed starch graft polyacrylic acid superabsorbent.
Embodiment 2
40g starch is added in the there-necked flask with agitator, reflux exchanger and thermometer, drip 60g distilled water, cooling stir gelatinization 5min in 55 ℃ of waters bath with thermostatic control after, obtain pasted starch.In addition, the KOH solution 100g that preparation massfraction is 35% adds Acrylic Acid Monomer 100g to make it neutralization in this solution, and degree of neutralization is 60%, is cooled to room temperature, obtains acrylate solution; The there-necked flask to 30 ℃ of pasted starch is housed with heating in water bath, add described acrylate solution, after stirring, the N of massfraction 0.05% successively, N '-methylene-bis acrylic acid amides solution 2g, the divinyl benzole soln 1g of massfraction 0.2%, continue to be warming up to 75 ℃, add the ammonium persulfate solution 5g of massfraction 0.5%, the ammonium sulfite solution 5g of massfraction 0.1%, stir 20min to reacting completely, obtain reaction product; Subsequently, reaction product is placed in to constant temperature oven, in 60 ℃, dry, pulverize, sieve; To obtaining resin surface after pulverizing, sieving, carry out secondary crosslinking processing, obtain starch graft polyacrylic acid superabsorbent.
Embodiment 3
40g starch is added in the there-necked flask with agitator, reflux exchanger thermometer, drip 60g distilled water, cooling stir gelatinization 10min in 50 ℃ of waters bath with thermostatic control after, obtain pasted starch.In addition, the KOH solution 120g that preparation massfraction is 20% adds Acrylic Acid Monomer 100g to make it neutralization in this solution, and degree of neutralization 50%, is cooled to room temperature, obtains acrylate solution; The there-necked flask to 45 ℃ of pasted starch is housed with heating in water bath, add described acrylate solution, after stirring, the N of massfraction 0.1% successively, N '-methylene-bis acrylic acid amides solution 1.5g, the divinyl benzole soln 1.5g of massfraction 0.1%, continue to be warming up to 70 ℃, add the ammonium persulfate solution 5g of massfraction 0.2%, the ammonium sulfite solution 5g of massfraction 0.3%, stir 30min to reacting completely, obtain reaction product; Subsequently, reaction product is placed in to constant temperature oven, in 70 ℃ dry, after pulverizing, sieving, obtain starch graft polyacrylic acid superabsorbent.
Embodiment 4
40g starch is added in the there-necked flask with agitator, reflux exchanger and thermometer, drip 60g distilled water, cooling stir gelatinization 10min in 80 ℃ of waters bath with thermostatic control after, obtain pasted starch.In addition, the KOH solution 120g that preparation massfraction is 20% adds Acrylic Acid Monomer 100g to make it neutralization in this solution, is cooled to room temperature, obtains acrylate solution; The there-necked flask to 60 ℃ of pasted starch is housed with heating in water bath, adds described acrylate solution, pass into nitrogen 8min, after stirring, add successively the ammonium persulfate solution 5g of massfraction 0.4% and the N of massfraction 0.4%, N
'-methylene-bis acrylic acid amides solution 0.1g, stirs 55min to reacting completely, and obtains reaction product; Subsequently, reaction product is placed in to constant temperature oven, in 80 ℃, dry, pulverize, sieve; To obtaining resin surface after pulverizing, sieving, carry out secondary crosslinking processing, obtain starch graft polyacrylic acid superabsorbent.
The performance index of the starch graft polyacrylic acid superabsorbent that the present invention makes are as shown in Table 1:
Table one
| Sample | Inhale 0.9% salt solution multiplying power (g/g) | Water-intake rate (g/g) | Biodegradability (resin is landfill 60d in pockets of soil) (%) |
| Embodiment 1 | 76.5 | 784 | 18.31 |
| Embodiment 2 | 79.1 | 815 | 20.47 |
| Embodiment 3 | 77.9 | 779 | 17.28 |
| Embodiment 4 | 78.3 | 829 | 22.45 |
Claims (4)
1. the preparation method of starch-grafted polymeric acrylic acid High hydrophilous resin, is characterized in that it is raw material that the method be take starch and vinylformic acid, comprises following steps:
subsequent disposal, is placed in constant temperature oven by reaction product, in 60 ℃-80 ℃ dry, after pulverizing, sieving, obtain starch graft polyacrylic acid superabsorbent.
2. the preparation method of starch-grafted polymeric acrylic acid High hydrophilous resin according to claim 1, is characterized in that step
middle gelatinization point is 55 ℃-60 ℃.
3. the preparation method of starch-grafted polymeric acrylic acid High hydrophilous resin according to claim 1, is characterized in that step
middle degree of neutralization is 40%-60%.
4. the preparation method of starch-grafted polymeric acrylic acid High hydrophilous resin according to claim 1, is characterized in that step
middlely after pulverizing, sieving, obtain starch graft polyacrylic acid superabsorbent surface and carry out secondary crosslinking processing.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103923261A (en) * | 2014-04-02 | 2014-07-16 | 合肥杰事杰新材料股份有限公司 | Preparation method of composite high-performance water-absorbing resin |
| CN104497212A (en) * | 2014-12-16 | 2015-04-08 | 广西大学 | Preparation method of bacteriostatic water-absorbent resin |
| CN104946261A (en) * | 2015-05-14 | 2015-09-30 | 和县正林苗木专业合作社 | Water-retaining agent for bamboo willow in drought regions |
| CN106188404A (en) * | 2016-07-24 | 2016-12-07 | 泉州海岸线新材料科技有限公司 | The formula of a kind of Technologies of Water-absorbing Resin: Corn Starch Grafting and preparation technology |
| CN112266302A (en) * | 2020-10-30 | 2021-01-26 | 安徽省农业科学院土壤肥料研究所 | Controlled release fertilizer and application thereof in rice cultivation |
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| CN1872890A (en) * | 2006-06-30 | 2006-12-06 | 上海华谊丙烯酸有限公司 | Method for preparing high absorptive resin in acrylic acid type |
| CN101045776A (en) * | 2007-04-20 | 2007-10-03 | 西北农林科技大学 | Method for synthesizing super absorbent resin from waxy wheat starch |
| CN101638459A (en) * | 2009-09-14 | 2010-02-03 | 内蒙古大学 | Method for preparing super absorbent resin with high potassium content by using carboxymethyl potato starch as raw material |
| CN101638456A (en) * | 2009-09-14 | 2010-02-03 | 内蒙古大学 | Method for preparing super absorbent resin with cross-linked structure by using potato starch as raw material |
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2013
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| WO2001089592A2 (en) * | 2000-05-25 | 2001-11-29 | Basf Aktiengesellschaft | Surface-treated superabsorbent polymer particles |
| CN1872890A (en) * | 2006-06-30 | 2006-12-06 | 上海华谊丙烯酸有限公司 | Method for preparing high absorptive resin in acrylic acid type |
| CN101045776A (en) * | 2007-04-20 | 2007-10-03 | 西北农林科技大学 | Method for synthesizing super absorbent resin from waxy wheat starch |
| CN101638459A (en) * | 2009-09-14 | 2010-02-03 | 内蒙古大学 | Method for preparing super absorbent resin with high potassium content by using carboxymethyl potato starch as raw material |
| CN101638456A (en) * | 2009-09-14 | 2010-02-03 | 内蒙古大学 | Method for preparing super absorbent resin with cross-linked structure by using potato starch as raw material |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103923261A (en) * | 2014-04-02 | 2014-07-16 | 合肥杰事杰新材料股份有限公司 | Preparation method of composite high-performance water-absorbing resin |
| CN103923261B (en) * | 2014-04-02 | 2019-03-05 | 合肥杰事杰新材料股份有限公司 | A kind of preparation method of composite high-performance water-absorbing resins |
| CN104497212A (en) * | 2014-12-16 | 2015-04-08 | 广西大学 | Preparation method of bacteriostatic water-absorbent resin |
| CN104946261A (en) * | 2015-05-14 | 2015-09-30 | 和县正林苗木专业合作社 | Water-retaining agent for bamboo willow in drought regions |
| CN106188404A (en) * | 2016-07-24 | 2016-12-07 | 泉州海岸线新材料科技有限公司 | The formula of a kind of Technologies of Water-absorbing Resin: Corn Starch Grafting and preparation technology |
| CN112266302A (en) * | 2020-10-30 | 2021-01-26 | 安徽省农业科学院土壤肥料研究所 | Controlled release fertilizer and application thereof in rice cultivation |
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Application publication date: 20140205 |