CN101935380B - Method for preparing potassium- and nitrogen-containing high water-absorbent resin from carboxymethyl potato starch serving as raw material - Google Patents
Method for preparing potassium- and nitrogen-containing high water-absorbent resin from carboxymethyl potato starch serving as raw material Download PDFInfo
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- CN101935380B CN101935380B CN2010105010054A CN201010501005A CN101935380B CN 101935380 B CN101935380 B CN 101935380B CN 2010105010054 A CN2010105010054 A CN 2010105010054A CN 201010501005 A CN201010501005 A CN 201010501005A CN 101935380 B CN101935380 B CN 101935380B
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Abstract
The invention discloses a method for preparing potassium- and nitrogen-containing high water-absorbent resin from carboxymethyl potato starch serving as a raw material. The product is prepared from the carboxymethyl potato starch serving as the raw material; and the carboxymethyl potato starch is water soluble, so compared with starch serving as the raw material, the carboxymethyl potato starch does not need gelatinization, and the preparation process is greatly simplified. Compared with like products, the high water-absorbent resin prepared by the method has the advantages of high water absorbing and retaining capability and high gel strength, contains potassium and nitrogen necessary for plant growth, and has great effects of resisting drought and keeping seedlings, increasing both production and income, promoting plant growth and the like for the soil in arid regions.
Description
Technical field
The present invention relates to be used for the preparation method of the High hydrophilous resin in fields such as agricultural gardening, desertification control, environment protection, civil engineering work, industrial goods, daily necessities; Refer in particular to carboxymethyl potato starch, vinylformic acid and N, N '-methylene-bisacrylamide is the method that main raw material prepares High hydrophilous resin.
Background technology
Water-absorbent that High hydrophilous resin is good and water-retentivity make it all obtain application in a lot of fields.High hydrophilous resin is joined in the soil, can change the crumb structure of soil, increase water-permeable, the ventilation property of soil, and can the water that add be stored, keep at the moisture of dry soil, the desert has tempting prospect aspect preventing and treating.Japan and France are used for the Middle East and North Africa with High hydrophilous resin now, implement the plan that the desert becomes the oasis.High hydrophilous resin is used for environment protection, can effectively removes the heavy metal ion in the sewage.High hydrophilous resin is applied to the physiological hygiene article can be effectively, rapid absorption urine and blood, therefore obtained widespread use in these fields.
The preparation method of High hydrophilous resin is a lot, and synthesis material is abundant, and production technique is different.Though China has obtained certain achievement in the research of High hydrophilous resin, and abroad to compare, gap is also quite big, and is low like the suction multiple of resin, salt resistant character is poor, the gel-strength after the suction is low, complex manufacturing, product cost are high.The kind of suitability for industrialized production manufacturer production and quantity are also fewer, have many need of work people deeply to do.We should give full play to the resourceful advantage of China's yam starch, produce the High hydrophilous resin of high-quality suitable China's national situation, lay the foundation for High hydrophilous resin becomes the third-largest agrochemicals of China and is applied to every field.
The High hydrophilous resin water-retaining capacity is extremely strong, and its suction back swelling is a gel, and when receiving the external force extruding, water also is difficult for running off, and has good water retention property.High hydrophilous resin is a kind of novel macromolecular material.High hydrophilous resin is born in the sixties in 20th century as a kind of functional high molecule material.Be described as one of new technology nineties in 20th century in Japan.The High hydrophilous resin of CMS preparation has advantages such as the multiplying power of absorption is high, speed is fast, so this series products has more wide application prospect.
Summary of the invention
It is the method that feedstock production contains potassium and nitrogen element High hydrophilous resin with the carboxymethyl potato starch that the technical problem that the present invention will solve provides a kind of; This preparation method is with carboxymethyl potato starch, vinylformic acid, acrylic amide, Pottasium Hydroxide, N; N '-methylene-bisacrylamide and persulphate etc. are raw material; Through reasonable proportioning, make High hydrophilous resin through the certain process process.
Technical problem of the present invention is solved by following scheme: be the method that feedstock production contains potassium and nitrogen element High hydrophilous resin with the carboxymethyl potato starch; It is characterized in that: carry out neutralization reaction with potassium hydroxide solution and the vinylformic acid of removing stopper; The mass ratio of carboxymethyl potato starch and vinylformic acid, acrylic amide, Pottasium Hydroxide is 1: 5-10: 5-10: 1.6-5.6; Vinylformic acid and potassium salt soln thereof after acrylamide soln, the neutralization are mixed with carboxymethyl potato starch; The persulphate that adds carboxymethyl potato starch quality 2.4%-3.4% is the N of initiator, 0.02%-0.1%; N '-methylene-bisacrylamide is made linking agent; Make mixture under agitation mix 0.5-1h, heating up gradually with heating in water bath afterwards reaches 65 ℃-80 ℃ until temperature, makes carboxymethyl potato starch and vinylformic acid and sodium salt thereof carry out graft copolymerization.Reaction process is carried out under nitrogen protection, and makes mixture under the boiling water bath condition, be incubated 1.5h, in baking oven, dries afterwards, pulverizes, and promptly gets High hydrophilous resin.
Technique scheme is said, and the vinylformic acid degree of neutralization of prepared High hydrophilous resin is 30%-90%, and its degree of neutralization can be 30%, 40%, 50%, 60%, 70%, 80%, 90%, and wherein most preferably condition is 50%-60%.
Technique scheme is said, and initiator potassium persulfate is 2.4%-3.4% (weight) with respect to the consumption of carboxymethyl potato starch, preferred 2.6%-3.2% (weight), most preferably 3.0%-3.2% (weight).
Technique scheme is said, linking agent N, and N '-methylene-bisacrylamide is 0.02%-0.1% (weight) with respect to the consumption of carboxymethyl potato starch, preferred 0.02%-0.1% (weight), most preferably 0.04%-0.06% (weight).
Technique scheme is said, and prepared High hydrophilous resin is inhaled amount of deionized water at 1400-1750 doubly.
Advantage of the present invention is: 1, this performance of products is fine; Inhale amount of deionized water doubly, inhale from the beginning the water yield and at 350-450 doubly inhale saline volume doubly at 100-120 at 1400-1750; Inhale artificial urine 60-80 doubly; Inhale artificial blood 100-150 doubly, compare with like product on the market, inhaling the pure water amount is about its twice.2, this product is raw material with the carboxymethyl potato starch; Because contain COOH and COONa structure in the carboxymethyl potato starch structure, the wetting ability of these groups is very strong, thereby the carboxymethyl potato starch water soluble; With use starch to compare not need gelatinization, simplified preparation technology greatly as raw material.3, contain necessary for plant growth potassium element and nitrogen element in this product, both can be used for soil moisture and keep, can increase soil nutrient again, have important use in farming, woods and gardening field and be worth.4, the proportioning raw materials among the present invention, acrylic acid degree of neutralization, dosage of crosslinking agent, initiator amount etc. all have different significantly, specific as follows with the technology of other products: the proportioning raw materials among (1) the present invention is meant ratio (monomer mass comprises the quality sum of vinylformic acid and acrylic amide) and the vinylformic acid of carboxymethyl potato starch and monomeric quality and the ratio of the quality of acrylic amide.Proportioning raw materials is one of important factor that influences water-intake rate.This is how many direct molecular weight that influence graftomer because of monomer content, thereby influences the water absorbing properties of product.In addition, the ratio of vinylformic acid and acrylic amide has direct influence to water-intake rate and product nitrogen content, and the acrylic amide consumption is too much; Because carboxamido-group is poorer than carboxylic acid group's wetting ability; Thereby the High hydrophilous resin water-intake rate that causes making descends, but the acrylic amide consumption is very few, thereby the High hydrophilous resin wetting ability increase that makes on the one hand causes being partly dissolved the resin water-intake rate is reduced; The product nitrogen content is low excessively on the other hand; Take all factors into consideration, final carboxymethyl potato starch and monomeric mass ratio are 1: 13-17, the mass ratio of vinylformic acid and acrylic amide are 1: 0.5-2.(2) acrylic acid degree of neutralization is the important factor that influences High hydrophilous resin water-intake rate and gel state, directly has influence on the height of High hydrophilous resin potassium content simultaneously.Consider that from reaction kinetics polymerizing acrylic acid receives the influence of pH value of solution value very big, is in the pH value at 2.4 o'clock, rate constant of polymerisation is about 5.8 * 106 (s-l), and when the pH value was 7.2, rate of polymerization descended 20 times approximately.Therefore low excessively as if degree of neutralization, in the reaction system-COOH content is higher, and polyreaction is wayward, is prone in the reaction process self-crosslinking takes place, and forms highly cross-linked low-molecular weight polymer, so water-intake rate is lower.When degree of neutralization increases, in the reaction system-the COOH major part is converted into-COOK, and-COOK is difficult for taking place self-crosslinking reaction, alleviated speed of response, degree of crosslinking is reduced, thereby water-intake rate is higher.But degree of neutralization is too high, in the resin-COOK content increases, and polymkeric substance wetting ability variation and cause water-intake rate to reduce.Take all factors into consideration, finally choosing degree of neutralization is 50%-60%.(3) select N for use, N '-methylene-bisacrylamide is a linking agent, can make High hydrophilous resin form bigger network behind the adding linking agent on the one hand; Help increasing water-intake rate; On the other hand, can increase the density of hydrophilic radical again, help the raising of water-intake rate equally.The effect of linking agent is to make the certain degree of crosslinking of formation between the macromolecular chain of carboxymethyl potato starch grafted propylene acid copolymer, makes the polymer formation fenestral fabric, thereby forms bigger three-dimensional suction space.When dosage of crosslinking agent increased, polymkeric substance internal crosslinking dot density increased, and the molecular resin chain-unfolding is restricted, network expansion difficulty during water absorption and swelling, and the amount that can hold water reduces, and the High hydrophilous resin water-intake rate reduces.Therefore adopting dosage of crosslinking agent is the 0.04%-0.06% of carboxymethyl potato starch quality.(4) initiator concentration increases, and the radical number increases in the system, has accelerated the speed of graft polymerization reaction, and the also corresponding increase of percentage of grafting is so water-intake rate increases; But initiator is excessive, and the polyradical of crossing of generation is prone to cause chain transfer and chain termination reaction, and percentage of grafting is descended; Be that grafted chain is difficult for increasing, polymericular weight is less, and reactive force is also little between macromole; Under the water molecules effect, can be partly dissolved, cause water-intake rate to descend.Therefore adopting initiator amount is the 3.0%-3.2% of carboxymethyl potato starch quality.
With the carboxymethyl potato starch is the synthetic super absorbent resin that contains potassium and nitrogen element of raw material; It not only has very high water regain; And contain necessary for plant growth potassium and nitrogen element; Will be applied to agriculture field widely, can solve the problem of lack of water dry proportion of crop planting lack of water and fertilizer, have huge social benefit and economic benefit.
Description of drawings
Fig. 1 is the process flow sheet of High hydrophilous resin
Fig. 2 is the influence curve of carboxymethyl potato starch and monomer mass comparison High hydrophilous resin water-intake rate
Fig. 3 is vinylformic acid and the acrylic amide mass ratio influence curve to the High hydrophilous resin water-intake rate
Fig. 4 is the influence curve of acrylic acid degree of neutralization to the High hydrophilous resin water-intake rate
Fig. 5 is the influence curve of initiator amount to the High hydrophilous resin water-intake rate
Fig. 6 is the influence curve of dosage of crosslinking agent to the High hydrophilous resin water-intake rate
Fig. 7 is the salt tolerance curve of High hydrophilous resin
Fig. 8 is the rate of water absorption curve of High hydrophilous resin
Fig. 9 is the liquid absorption of High hydrophilous resin in different liqs
Figure 10 is the infrared spectrogram of High hydrophilous resin
Embodiment
Embodiment 1: weighing 6.8g Pottasium Hydroxide, measure the 30.0ml deionized water, the preparation potassium hydroxide solution, under ice-water bath cooling and stirring condition, in remove the vinylformic acid of stopper with 17.5g.Take by weighing the 17.5g acrylic amide, with the 35.0ml deionized water it is dissolved, acrylamide soln that dissolving is good and 2.5g carboxymethyl potato starch mix it in stirring at room 1h.The vinylformic acid of becoming reconciled in the adding, 80mg Potassium Persulphate initiator, 1.0mgN, N '-methylene-bisacrylamide stirs heating down; Control rate of heating simultaneously; Bath temperature is slowly raise, graft copolymerization is fully carried out, after graft copolymerization begins, stop to stir.After this heat up gradually, after reaching the boiling water bath temperature, continue heating and make it, stop logical nitrogen, be cooled to room temperature at this TR internal reaction 1.5h.Product is taken out, after drying, pulverizing, get the white granular High hydrophilous resin.The suction deionized water rate of this product is 1650g/g.
Embodiment 2: weighing 7.3g Pottasium Hydroxide, measure the 30.0ml deionized water, the preparation potassium hydroxide solution, under ice-water bath cooling and stirring condition, in remove the vinylformic acid of stopper with 18.7g.Take by weighing the 18.7g acrylic amide, with the 35.0ml deionized water it is dissolved, acrylamide soln that dissolving is good and 2.5g carboxymethyl potato starch mix it in stirring at room 1h.The vinylformic acid of becoming reconciled in the adding, 80mg Potassium Persulphate initiator, 1.0mgN, N '-methylene-bisacrylamide stirs heating down; Control rate of heating simultaneously; Bath temperature is slowly raise, graft copolymerization is fully carried out, after graft copolymerization begins, stop to stir.After this heat up gradually, after reaching the boiling water bath temperature, continue heating and make it, stop logical nitrogen, be cooled to room temperature at this TR internal reaction 1.5h.Product is taken out, after drying, pulverizing, get the white granular High hydrophilous resin.The suction deionized water rate of this product is 1680g/g.
Embodiment 3: weighing 7.8g Pottasium Hydroxide, measure the 30.0ml deionized water, the preparation potassium hydroxide solution, under ice-water bath cooling and stirring condition, in remove the vinylformic acid of stopper with 20.0g.Take by weighing the 20.0g acrylic amide, with the 35.0ml deionized water it is dissolved, acrylamide soln that dissolving is good and 2.5g carboxymethyl potato starch mix it in stirring at room 1h.The vinylformic acid of becoming reconciled in the adding, 80mg Potassium Persulphate initiator, 1.0mgN, N '-methylene-bisacrylamide stirs heating down; Control rate of heating simultaneously; Bath temperature is slowly raise, graft copolymerization is fully carried out, after graft copolymerization begins, stop to stir.After this heat up gradually, after reaching the boiling water bath temperature, continue heating and make it, stop logical nitrogen, be cooled to room temperature at this TR internal reaction 1.5h.Product is taken out, after drying, pulverizing, get the white granular High hydrophilous resin.The suction deionized water rate of this product is 1600g/g.
Embodiment 4: weighing 4.9g Pottasium Hydroxide, measure the 30.0ml deionized water, the preparation potassium hydroxide solution, under ice-water bath cooling and stirring condition, in remove the vinylformic acid of stopper with 12.5g.Take by weighing the 25.0g acrylic amide, with the 35.0ml deionized water it is dissolved, acrylamide soln that dissolving is good and 2.5g carboxymethyl potato starch mix it in stirring at room 1h.The vinylformic acid of becoming reconciled in the adding, 80mg Potassium Persulphate initiator, 1.0mgN, N '-methylene-bisacrylamide stirs heating down; Control rate of heating simultaneously; Bath temperature is slowly raise, graft copolymerization is fully carried out, after graft copolymerization begins, stop to stir.After this heat up gradually, after reaching the boiling water bath temperature, continue heating and make it, stop logical nitrogen, be cooled to room temperature at this TR internal reaction 1.5h.Product is taken out, after drying, pulverizing, get the white granular High hydrophilous resin.The suction deionized water rate of this product is 1650g/g.
Embodiment 5: weighing 8.7g Pottasium Hydroxide, measure the 30.0ml deionized water, the preparation potassium hydroxide solution, under ice-water bath cooling and stirring condition, in remove the vinylformic acid of stopper with 22.5g.Take by weighing the 15.0g acrylic amide, with the 35.0ml deionized water it is dissolved, acrylamide soln that dissolving is good and 2.5g carboxymethyl potato starch mix it in stirring at room 1h.The vinylformic acid of becoming reconciled in the adding, 80mg Potassium Persulphate initiator, 1.0mgN, N '-methylene-bisacrylamide stirs heating down; Control rate of heating simultaneously; Bath temperature is slowly raise, graft copolymerization is fully carried out, after graft copolymerization begins, stop to stir.After this heat up gradually, after reaching the boiling water bath temperature, continue heating and make it, stop logical nitrogen, be cooled to room temperature at this TR internal reaction 1.5h.Product is taken out, after drying, pulverizing, get the white granular High hydrophilous resin.The suction deionized water rate of this product is 1670g/g.
Embodiment 6: acrylic acid Pottasium Hydroxide consumption that neutralizes is 8.7g, and other experiment conditions are identical with the condition of embodiment 2, and the suction deionized water rate of product is 1690g/g.
Embodiment 7: acrylic acid Pottasium Hydroxide consumption that neutralizes is 10.2g, and other experiment conditions are identical with the condition of embodiment 2, and the suction deionized water rate of product is 1660g/g.
Embodiment 8: initiator amount is 70mg, and other experiment conditions are identical with the condition of embodiment 6, and the suction deionized water rate of product is 1660g/g.
Embodiment 9: initiator amount is 75mg, and other experiment conditions are identical with the condition of embodiment 6, and the suction deionized water rate of product is 1710g/g.
Embodiment 10: dosage of crosslinking agent is 1.5mg, and other experiment conditions are identical with the condition of embodiment 9, and the suction deionized water rate of product is 1700g/g.
Embodiment 10: dosage of crosslinking agent is 2.0mg, and other experiment conditions are identical with the condition of embodiment 9, and the suction deionized water rate of product is 1605g/g.
The ir spectra of High hydrophilous resin uses NEXUSTM 670FT-IR E.S.P type IR, is measured by University of the Inner Mongol.Product with embodiment 9 is an example, the main absorption peak of IR spectrum: 3447cm
-1Stretching vibration absorption peak for-OH; 3125cm
-1Stretching vibration absorption peak for NH; 1633cm
-1Folded honeybee for asymmetrical stretching vibration absorption peak and the acid amides C=O stretching vibration absorption peak of carboxylate salt COO-; 1401cm
-1Symmetrical stretching vibration peak for carboxylate salt COO-.Measure through German Elementar Vario ELIII type ultimate analysis instrument, carbon, hydrogen and the nitrogen element content of embodiment 9 products are respectively: C%=40.49, H%=6.070, N%=7.218.Potassium element content through atomic absorption spectroscopy determination instance 9 products is: K%=12.5.
Claims (5)
1. be the method that feedstock production contains potassium and nitrogen element High hydrophilous resin with the carboxymethyl potato starch, it is characterized in that: under the ice-water bath cooling, carry out neutralization reaction with potassium hydroxide solution and the vinylformic acid of removing stopper; Wherein the mass ratio of carboxymethyl potato starch and vinylformic acid, Pottasium Hydroxide is 1: 5-10: 1.6-5.6, and the mass ratio of vinylformic acid and acrylic amide is 1: 0.5-2, with the vinylformic acid after acrylamide soln, the neutralization and sylvite and carboxymethyl potato starch mixing; The Potassium Persulphate that adds carboxymethyl potato starch quality 2.4%-3.4% is made initiator, the N of 0.02%-0.1%, and N '-methylene-bisacrylamide is made linking agent; Stirred 0.5-1.0 hour, mixture is under agitation mixed, then under nitrogen protection; Heating in water bath also stirs, and stops to stir in boiling water bath insulation reaction 1-2 hour when reaching certain temperature; Stop logical nitrogen then, product is taken out, cut into fritter; In 40 ℃-60 ℃ baking oven, dry; Pulverize, promptly get the High hydrophilous resin that contains potassium and nitrogen element, prepared High hydrophilous resin is inhaled amount of deionized water at 1400-1750 doubly.
2. method according to claim 1 is characterized in that: the grafting parent of employing is a carboxymethyl potato starch, and promptly yam starch is handled through carboxymethylation, and the grafted monomer of employing is the mix monomer of vinylformic acid and acrylic amide.
3. method according to claim 1 is characterized in that: the vinylformic acid degree of neutralization optimal conditions of prepared High hydrophilous resin is between 50%-60%.
4. method according to claim 1 is characterized in that: initiator potassium persulfate with respect to the optimal conditions of carboxymethyl potato starch consumption in 3.0%-3.2% (weight).
5. method according to claim 1 is characterized in that: linking agent N, N '-methylene-bisacrylamide with respect to the optimal conditions of carboxymethyl potato starch consumption between 0.04%-0.06% (weight).
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Families Citing this family (9)
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| CN103360503A (en) * | 2013-05-23 | 2013-10-23 | 内蒙古大学 | New process for preparing super absorbent resin by graft copolymerization of carboxymethyl potato starch ether sodium |
| CN103342779B (en) * | 2013-05-23 | 2016-03-30 | 内蒙古大学 | Carboxymethyl potato starch ether sodium prepares the novel process of High hydrophilous resin |
| CN104072670B (en) * | 2014-07-07 | 2018-04-06 | 内蒙古大学 | The method that carboxymethyl potato slag prepares nitrogenous potassium high hydroscopic resin |
| CN104086708B (en) * | 2014-07-08 | 2016-11-23 | 内蒙古大学 | Carboxymethyl Receptaculum Helianthi prepares nitrogenous and potassium High hydrophilous resin method |
| CN105713139B (en) * | 2015-05-20 | 2021-06-01 | 内蒙古大学 | Novel process for preparing high-potassium-content super absorbent resin by taking carboxymethyl potato starch and acrylamide as raw materials |
| CN105732898A (en) * | 2015-05-20 | 2016-07-06 | 内蒙古大学 | Novel process of producing super absorbent resin from carboxymethyl potato starch and acrylamide as raw materials |
| CN106146737A (en) * | 2015-05-20 | 2016-11-23 | 内蒙古大学 | The method preparing super absorbent resin with high potassium content for raw material one kettle way with carboxymethyl potato starch and hydrogen peroxide |
| CN109705874A (en) * | 2018-12-28 | 2019-05-03 | 北京城市之光生态环境有限公司 | A kind of water-loss reducer of soil and preparation method thereof |
| CN115920858A (en) * | 2022-12-05 | 2023-04-07 | 四川省遂宁生态环境监测中心站 | Swelling resin heavy metal adsorbent and preparation method thereof |
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| CN101638461A (en) * | 2009-09-14 | 2010-02-03 | 内蒙古大学 | Method for synthesizing super absorbent resin containing phosphorus and nitrogen by graft copolymerization reaction of potato starch organic phosphate |
| CN101638458A (en) * | 2009-09-14 | 2010-02-03 | 内蒙古大学 | Method for preparing super absorbent resin by using carboxymethyl potato starch as raw material |
| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101638461A (en) * | 2009-09-14 | 2010-02-03 | 内蒙古大学 | Method for synthesizing super absorbent resin containing phosphorus and nitrogen by graft copolymerization reaction of potato starch organic phosphate |
| CN101638458A (en) * | 2009-09-14 | 2010-02-03 | 内蒙古大学 | Method for preparing super absorbent resin by using carboxymethyl potato starch as raw material |
| 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 |
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Effective date of registration: 20161215 Address after: 530022 the Guangxi Zhuang Autonomous Region Nanning Qingxiu District National Road No. 93 Xinxing Hotel, 19 storey office building A2, room A3 Patentee after: Guangxi Shen letter Technology Co. Ltd. Address before: 010021 Hohhot West Road, the Inner Mongolia Autonomous Region, No. 235 Patentee before: Inner Mongolia University |