CN101985486B - Method for preparing super absorbent resin containing compound plant growth regulator - Google Patents

Method for preparing super absorbent resin containing compound plant growth regulator Download PDF

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Publication number
CN101985486B
CN101985486B CN2010105013071A CN201010501307A CN101985486B CN 101985486 B CN101985486 B CN 101985486B CN 2010105013071 A CN2010105013071 A CN 2010105013071A CN 201010501307 A CN201010501307 A CN 201010501307A CN 101985486 B CN101985486 B CN 101985486B
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China
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starch
plant growth
growth regulator
high hydrophilous
hydrophilous resin
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CN101985486A (en
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温国华
林波
申洋洋
朱如月
目仁更
张伟
李东芳
张媛
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Inner Mongolia University
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Inner Mongolia University
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  • Soil Conditioners And Soil-Stabilizing Materials (AREA)

Abstract

The invention provides a method for preparing a super absorbent resin containing a compound plant growth regulator. In the method, sodium fulvate and nitrophenolate are added in a reaction system for polymerization before graft copolymerization of starch or starch derivatives, crylic acid and other monomers, and the absorbent times of the prepared super absorbent resin is 340-700. The method in the invention has the advantages of simple synthesis process, no pollution and low production cost, and the prepared product contains the sodium fulvate and nitrophenolate with the function of plant growth regulation, and can be widely used in the fields of agriculture, forestry, desertification control, gardening and the like.

Description

A kind of preparation method who contains the composite plant growth regulator High hydrophilous resin
Technical field
The present invention relates to a kind of preparation method of High hydrophilous resin, particularly relate to a kind of preparation method who contains the composite plant growth regulator High hydrophilous resin, this product can be widely used in fields such as agricultural, forestry, gardening and desertification control.
Background technology
Super absorbent resin all has important use, especially being most widely used in fields such as farming, woods, gardening and desertification controls in a lot of fields with the suction and the water retention property of its excellence.Super absorbent resin often is used to soil improvement, desert afforestation, soilless culture, drought-resistant water-preserving, agriculture chemical slowly-releasing etc. on agricultural.High hydrophilous resin is joined in the soil, the structure of can improving the soil, increase the suction and the water retention capacity of soil, improve soil water regime, regulate the triphasic distribution of solid, liquid, gas in the soil, improve the regulating power of soil to temperature, also provide enabling environment simultaneously for the procreation of soil microorganisms, its activity is improved greatly, help the absorption of plant to nutritive element, can obviously improve seed germination rate, promote growth and development of plants, for the output that improves farming, woods, gardening, vegetables, fruit tree, pasture and water has been created good condition.
Along with High hydrophilous resin is constantly expanded in the range of application in fields such as agroforestry, common High hydrophilous resin can not satisfy application requiring on performance and function, the high-performance High hydrophilous resin that R and D can be satisfied the specified property requirement has become current focus.The particularly application aspect farming, woods and gardening presses for the practical more multifunctional type High hydrophilous resin of development, as contains novel super absorbent resins such as plant-growth nutritive element, slow release fertilizer.
SODLUM FULVATE and o/p-nitrophenol sodium all are the broad spectrum type plant-growth regulator; all be widely used in agricultural and field such as gardening, advantages such as they have, and the cellular plasm of promotion flows, improves cell viability, quickens vine growth and development, short root strong sprout, flower and fruit protecting, raising output, enhancing anti-adversity ability.SODLUM FULVATE and o/p-nitrophenol sodium are incorporated in the High hydrophilous resin, make High hydrophilous resin except that having the water-absorbing-retaining performance, also have the plant growth regulating function, enlarged the range of application of High hydrophilous resin, make it have more practical value.
Summary of the invention
The purpose of this invention is to provide the preparation method who contains the composite plant growth regulator High hydrophilous resin that use in fields such as a kind of suitable farming, woods, desertification control and gardening.
Technical scheme of the present invention is as follows: under the ice-water bath cooling and stirring, remove the vinylformic acid of stopper with sodium hydroxide or potassium hydroxide solution neutralization, obtain vinylformic acid and salts solution thereof, afterwards with starch derivative or hot gelatinization after starch, acrylamide, SODLUM FULVATE and o/p-nitrophenol sodium solution, linking agent N, N '-methylene-bisacrylamide solution and initiator potassium persulfate are mixed, at room temperature stir 0.5-1.0h, it is mixed, wherein raw material mass mixture ratio is 1 part of starch or starch derivative, 0.168-6.990 part sodium hydroxide or 0.47-9.80 part potassium hydroxide, 3-14 part vinylformic acid, 0-20 part acrylamide, 0.0004-0.4 part SODLUM FULVATE, 0.0004-1.0961 part o/p-nitrophenol sodium, 0.00002-0.04000 part N, N '-methylene-bisacrylamide, 0.005-0.050 part Potassium Persulphate, 20-40 part deionized water feeds nitrogen and slowly heating in water-bath then, makes it react 1h down at 60-80 ℃, continue to heat up, in boiling water bath, be incubated 1-2h again, stop logical nitrogen, be cooled to room temperature, product is taken out, oven dry, pulverize, sieve, promptly get the High hydrophilous resin that contains composite plant growth regulator, the suction multiple of product is 340-700 times.
Starch described in the technique scheme is yam starch, W-Gum, tapioca (flour), starch derivative is carboxymethyl starch, phosphate ester starch, cross-linking starch, acetate starch, sulphur ortho ester starch, pre-gelatinized starch, preferred yam starch or yam starch derivative.
The described acrylic acid degree of neutralization of scheme is 20%, 30%, 35%, 40%, 45%, 50%, 55%, 60%, 70%, 80%, preferred 30%-60%.
Deionized water in the described proportioning raw materials of scheme is the used deionized water total amount of dissolved hydrogen sodium oxide or the hot gelatinization of potassium hydroxide, acrylamide, SODLUM FULVATE, o/p-nitrophenol sodium and starch.
Advantage of the present invention is as follows:
(1) the prepared product of the present invention also contains the SODLUM FULVATE and the o/p-nitrophenol sodium of trophic function except that the water-absorbing-retaining performance with High hydrophilous resin.
(2) the present invention uses starch or starch derivative as parent, can significantly reduce production costs, and this product has easy degraded, free of contamination advantage.
(3) the present invention adopts one-step synthesis, and production technique is simple, and the no three wastes produce, and help industrialization production.
Description of drawings
Fig. 1 is preparation technology's schema of product
Fig. 2 is the infrared spectrogram of embodiment 4 products
Embodiment
Embodiment 1: with 15ml deionized water dissolving 5.0g sodium hydroxide, under the ice-water bath cooling and stirring, in and 30g (28.6ml) vinylformic acid; With 6ml deionized water dissolving 0.01g sodium onitrophenol, 0.01g Sodium p-nitrophenoxide and 0.1g SODLUM FULVATE; Taking by weighing the 5.0g yam starch is dissolved in the 25ml deionized water, heat gelatinization 1-2 minute down at 60-70 ℃, be cooled to after the room temperature with in the vinylformic acid and the salts solution thereof of becoming reconciled, SODLUM FULVATE, o/p-nitrophenol sodium solution, the 80mg Potassium Persulphate, 4ml concentration is the N of 5mg/ml, N '-methylene-bisacrylamide solution mixes, at room temperature stir 0.5h, feed nitrogen then and slowly heating in water-bath, make it react 1h down at 60-75 ℃, continue to heat up, in boiling water bath, be incubated 1.5h again, stop logical nitrogen, be cooled to room temperature, product is taken out, oven dry, pulverize, sieve, promptly get the High hydrophilous resin that contains composite plant growth regulator, the suction multiple of present embodiment products obtained therefrom is 475 times.
Embodiment 2: with 27ml deionized water dissolving 8.33g sodium hydroxide, under the ice-water bath cooling and stirring, in and 30g (28.6ml) vinylformic acid; With 35ml deionized water dissolving 0.1g o-NP, 0.2g p-NP and 0.3g SODLUM FULVATE, the vinylformic acid and the salts solution thereof of becoming reconciled in adding then, 2.5g carboxymethyl potato starch, 8ml concentration is the N of 5mg/ml, and N '-methylene-bisacrylamide solution and 65mg Potassium Persulphate at room temperature stir 0.5h, feed nitrogen then and begin slow heating, make it react 1h down, continue to heat up, in boiling water bath, be incubated 1-2h again at 60-80 ℃, stop logical nitrogen, be cooled to room temperature, product is taken out, oven dry, pulverize, sieve, promptly get the High hydrophilous resin that contains composite plant growth regulator, the suction multiple of present embodiment products obtained therefrom is 660 times.
Embodiment 3: experiment condition is with embodiment 2, and different is that the suction multiple of present embodiment products obtained therefrom is 610 times with 35ml deionized water dissolving 0.01g o-NP, 0.01g p-NP and 0.3g SODLUM FULVATE.
Embodiment 4: experiment condition is with embodiment 2, and different is that the suction multiple of present embodiment products obtained therefrom is 675 times with 35ml deionized water dissolving 0.05g o-NP, 0.05g p-NP and 0.3g SODLUM FULVATE.
Embodiment 5: experiment condition is with embodiment 2, and different is that the suction multiple of present embodiment products obtained therefrom is 655 times with 35ml deionized water dissolving 0.1g o-NP, 0.1g p-NP and 0.3g SODLUM FULVATE.
Embodiment 6: experiment condition is with embodiment 2, and different is that the suction multiple of present embodiment products obtained therefrom is 390 times with 35ml deionized water dissolving 0.2g o-NP, 0.2g p-NP and 0.3g SODLUM FULVATE.
Embodiment 7: with 24ml deionized water dissolving 6.5g potassium hydroxide, under the ice-water bath cooling and stirring, in and 28g (26.7ml) vinylformic acid; With 40ml deionized water dissolving dissolving 0.05g o-NP, 0.05g p-NP and 0.5g SODLUM FULVATE, then with in the vinylformic acid and the salts solution thereof of becoming reconciled, 2.5g phosphoric acid ester yam starch, the 7g acrylamide, 6ml concentration is the N of 5mg/ml, and N '-methylene-bisacrylamide solution and 100mg Potassium Persulphate mix, and at room temperature stir 0.5h, feed nitrogen then and begin slow heating, make it react 1h down, continue to heat up, in boiling water bath, be incubated 1-2h again at 70-80 ℃, stop logical nitrogen, be cooled to room temperature, product is taken out, oven dry, pulverize, sieve, promptly get the High hydrophilous resin that contains composite plant growth regulator, the suction multiple of present embodiment products obtained therefrom is 605 times.
Embodiment 8: experiment condition is with embodiment 7, and different is that the suction multiple of present embodiment products obtained therefrom is 340 times with 40ml deionized water dissolving 0.05g o-NP, 0.05g p-NP and 0.01g SODLUM FULVATE.
Embodiment 9: experiment condition is with embodiment 7, and different is that the suction multiple of present embodiment products obtained therefrom is 400 times with 40ml deionized water dissolving 0.05g o-NP, 0.05g p-NP and 0.05g SODLUM FULVATE.
Embodiment 10: experiment condition is with embodiment 7, and different is that the suction multiple of present embodiment products obtained therefrom is 385 times with 40m1 deionized water dissolving 0.05g o-NP, 0.05g p-NP and 0.1g SODLUM FULVATE.
Embodiment 11: experiment condition is with embodiment 7, and different is that the suction multiple of present embodiment products obtained therefrom is 700 times with 40ml deionized water dissolving 0.05g o-NP, 0.05g p-NP and 0.7g SODLUM FULVATE.
The infrared spectra of embodiment 7 products is by NEXUS TM670FT-IR E.S.P type determination of infrared spectroscopy.Measure through German Elementar Vario ELIII type ultimate analysis instrument, the constituent content of embodiment 7 products is: C%=40.09, H%=5.867, N%=3.110.

Claims (5)

1. preparation method who contains the composite plant growth regulator High hydrophilous resin, it is characterized in that: under the ice-water bath cooling and stirring, remove the vinylformic acid of stopper with sodium hydroxide or potassium hydroxide solution neutralization, obtain vinylformic acid and salts solution thereof, afterwards with starch derivative or hot gelatinization after starch, acrylamide, SODLUM FULVATE and sodium onitrophenol or p-NP sodium solution, linking agent N, N '-methylene-bisacrylamide solution and initiator potassium persulfate are mixed, at room temperature stir 0.5-1.0h, it is mixed, wherein raw material mass mixture ratio is 1 part of starch or starch derivative, 0.168-6.990 part sodium hydroxide or 0.47-9.80 part potassium hydroxide, 3-14 part vinylformic acid, 0-20 part acrylamide, 0.0004-0.4 part SODLUM FULVATE, 0.0004-1.0961 part sodium onitrophenol or Sodium p-nitrophenoxide, 0.00002-0.04000 part N, N '-methylene-bisacrylamide, 0.005-0.050 part Potassium Persulphate, 20-40 part deionized water, feed nitrogen then and slowly heating in water-bath, make it react 1h down, continue to heat up, in boiling water bath, be incubated 1-2h again at 60-80 ℃, stop logical nitrogen, be cooled to room temperature, product is taken out, oven dry, pulverize, sieve, promptly get the High hydrophilous resin that contains composite plant growth regulator, the suction multiple of product is 340-700 times.
2. a kind of preparation method who contains the composite plant growth regulator High hydrophilous resin according to claim 1 is characterized in that: used starch is yam starch, W-Gum, tapioca (flour).
3. a kind of preparation method who contains the composite plant growth regulator High hydrophilous resin according to claim 1 is characterized in that: used starch derivative is carboxymethyl starch, phosphate ester starch, cross-linking starch, acetate starch, sulphur ortho ester starch.
4. a kind of preparation method who contains the composite plant growth regulator High hydrophilous resin according to claim 1 is characterized in that: used starch or starch derivative are yam starch or yam starch derivative.
5. a kind of preparation method who contains the composite plant growth regulator High hydrophilous resin according to claim 1 is characterized in that: acrylic acid degree of neutralization is 30%-60%.
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CN2010105013071A 2010-10-09 2010-10-09 Method for preparing super absorbent resin containing compound plant growth regulator Expired - Fee Related CN101985486B (en)

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CN102775555B (en) * 2012-08-15 2013-08-07 内蒙古大学 Method for synthesizing high water absorbent polymer by using potato starch xanthate and acrylamide
CN105859966B (en) * 2016-04-14 2018-10-19 安徽农业大学 A kind of super absorbent resin and preparation method thereof containing Zn-ef ficiency
CN105859967B (en) * 2016-04-14 2019-01-15 安徽农业大学 A kind of super absorbent resin and preparation method thereof containing iron ion
CN105732900B (en) * 2016-04-14 2018-12-18 安徽农业大学 A kind of super absorbent resin and preparation method thereof containing boron element
CN107118778A (en) * 2017-06-14 2017-09-01 合肥助航生态农业科技有限公司 Water-loss reducer of soil and preparation method thereof
CN113322073B (en) * 2021-04-30 2022-07-01 上海工程技术大学 Degradable dendritic soil conditioner and preparation method thereof

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US4997581A (en) * 1988-11-14 1991-03-05 Nalco Chemical Company Additive and method for temporarily reducing permeability of subterranean formations
CN1319618A (en) * 2001-02-27 2001-10-31 北京市朝阳区科龙达新技术应用研究所 Holoside water retaining agent and preparation method thereof
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