CN101429077A - Process for producing ultra-high salt supported hydrogel - Google Patents
Process for producing ultra-high salt supported hydrogel Download PDFInfo
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- CN101429077A CN101429077A CNA2008102194010A CN200810219401A CN101429077A CN 101429077 A CN101429077 A CN 101429077A CN A2008102194010 A CNA2008102194010 A CN A2008102194010A CN 200810219401 A CN200810219401 A CN 200810219401A CN 101429077 A CN101429077 A CN 101429077A
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Abstract
The invention discloses a method for preparing an ultrahigh saline loaded aquagel. The method is to polymerize a saline solution, a mixed solution of an organic monomer and a cross-linking agent and an aqueous solution of an evocating agent through one-step polymerization to obtain the ultrahigh saline load aquagel, and successfully store both salt and water in a high-molecular gel network structure so as to realize integrated regulation and control of the water and the salt. The method selects proper cross-linking agent and organic monomer, so when the aquagel is applied to preparing gel state fertilizer for integrally controlling release of fertilizer and water, soluble salt exists in the aquagel in a mode of molecules or ions, and based on diffusion penetration principle, the cross-linking agent and the monomer can sustainably supply moisture, nutritive ingredients of nitrogen, phosphor and kalium and other plant required nutritive elements for plants. The gel state fertilizer prepared by the method is convenient to produce and apply, has good effect of moisture and fertility preservation, lower cost than a common water retention agent and great reduction of controlled release fertilizer, and has good application prospect to horticultural cultivation, drought resistance and seedling protection, desert reformation and other aspects.
Description
Technical field
The invention belongs to the control release technic field, relate to the preparation method of the integrated controlled release system body of soluble salt and water, specifically about the preparation method of the hydrogel of superelevation salt (chemical fertilizer) load of the integrated regulation and control of liquid manure.
Background technology
Chemical fertilizer mostly is inorganic soluble salt, in order to improve its utilization ratio, and reduces because of the use of the chemical fertilizer pollution to atmosphere, soil, underground water and rivers, lake, and in nearly decades, the controlled-release technology of fertilizer obtains active research and exploitation.Using film-coating technique formation coating controlled-release fertilizer is the technology of studying at most, expectation reaches the release rate of realization chemical fertilizer and the suitable purpose of absorption rate of plant by selecting the means such as thickness, porosity, degradation speed and size of coating film material, controlling packet overlay film.
Coated release-controlled primary process is: (1) free moisture sees through coating; (2) the moisture dissolving chemical fertilizer through coating forms solution; (3) fertilizer solution diffuses out coating, enters soil, is made for thing and absorbs.Therefore the existence of external water source is the coated release-controlled technology prerequisite that plays a role.The desert and the desert area of, soil depletion short of rain in arid, coat fertilizer just is difficult to play a role.Owing to the restriction of factors such as cost and price, coating controlled-release fertilizer does not also obtain bigger popularization except being applied in the arable farming of higher gears such as gardening simultaneously.
Gel has very strong water-absorbing-retaining function, being stored in wherein liquid can spread lentamente when contacting with porous mass and discharge, and the speed that discharges can perhaps be selected different function monomers to regulate parameters such as the functional structure of gel, network density or intensity and control by changing linking agent kind, consumption.The gel of being reported at present is that xerogel is immersed in the solution of corresponding chemical material to the load of chemical substance basically, make solution enter gel network by infiltration, expanded balloon is carried out that drying makes, charge capacity is not high to be the main weak point of this method again.
Above-mentioned characteristic according to gel, the applicant considers the fertilizer solution of high density is stored in the gel, realize water, fertile integrated, and it is suitable with plant absorbing speed with the nutriment in a fertilizer release rate to reach moisture by adjusting gel structure parameter, if can realize, use this gel state fertilizer, make the controlled-release technology of fertilizer obtain active research, develop and promote the use of, especially can solve the purpose that plant nutrition is realized continuing slowly to supply with in arid place short of rain.Do not see at present the preparation method's of ultra-high salt supported hydrogel correlation technique report.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, provide a kind of water, fertile integrated, use conveniently, the fertile preparation method of gel state short of rain, barren in arid and superelevation salt (chemical fertilizer) load that the Desert Area result of use is good, solved high chemical fertilizer charge capacity and the incorporate key technical problem of liquid manure, preparing a kind of ultra-high salt supported hydrogel is novel gel state fertilizer.
Of the present inventionly be achieved by following technical solution:
A kind of preparation method of ultra-high salt supported hydrogel is provided, obtains described ultra-high salt supported hydrogel by the one-step polymerization method reaction after preparing the aqueous solution of required salts solution, organic monomer and linking agent mixed solution, initiator, specifically may further comprise the steps:
(1) with the water-soluble preparation salts solution of soluble salt;
(2) with in organic monomer and the high salt concentration solution that joins step (1) preparation after linking agent mixes, make and treat polymeric solution; And adopt inert atmosphere protection to treat polymerization system, hierarchy of control temperature;
(3) initiator is made the aqueous solution, what join that step (2) makes treats that in the polymeric solution, polyreaction obtains ultra-high salt supported hydrogel.
The described soluble salt of step (1) is the soluble salt that contains plant desired nutritional element arbitrarily that use this area, compounding high concentration salts solution of the present invention.
The described inert atmosphere of step (2) can be by any one gas atmosphere in nitrogen, argon gas or the carbonic acid gas; Hierarchy of control temperature is 10～90 ℃.
Described organic monomer of step (2) and the linking agent mass percent in the described salts solution of step (1) is 1～20%; Linking agent is 1:10～1:5 with the ratio of the amount of organic monomer.
Described organic monomer is selected from following compound: vinylformic acid, α-Jia Jibingxisuan, acrylamide, vinylbenzene, alpha-methyl styrene, vinyl acetate between to for plastic, p-sulfonic acid vinylbenzene, Hydroxyethyl acrylate, α-Jia Jibingxisuan hydroxyl ethyl ester, Propylene glycol monoacrylate or α-Jia Jibingxisuan hydroxypropyl acrylate.
When organic monomer was selected vinylformic acid or α-Jia Jibingxisuan for use, the carboxyl of vinylformic acid or α-Jia Jibingxisuan needed with the alkali neutralization, and used alkali is sodium hydroxide, potassium hydroxide, calcium hydroxide, ammonium hydroxide or hydrated barta, and the degree of neutralization of carboxyl is 10～100%.
Described linking agent is selected from following compound: ethylene glycol diacrylate, glycol methacrylate, methylene-bisacrylamide, ethylenebis acrylamide, glycidyl acrylate or α-Jia Jibingxisuan glycidyl ester.
The initiator weight percentage is 5～30% in the aqueous solution of the described initiator of step (3), and the consumption of initiator is controlled to be 0.5～5% of organic monomer total mass.
Described initiator is one or more the mixture of arbitrary proportion in ceric sulfate, hydrogen peroxide, ammonium persulphate, Potassium Persulphate, ammonium cerous sulfate, ferrous sulfate, sodium bisulfite or the S-WAT.
The condition of the described polyreaction of step (3) is conditions such as the described system temperature of step (2), inertia, described system temperature is controlled to be 10～90 ℃, described inert atmosphere can be by any one or the multiple gases atmosphere in nitrogen, argon gas or the carbonic acid gas, polymerase 10 .5～5 hour.
Preparation method of the present invention can be applicable to prepare salt and water integrated controlled release preparation, especially is applied to prepare the gel state fertilizer of chemical fertilizer and water integrated controlled release.
The difference of ultra-high salt supported hydrogel that the inventive method prepares and traditional water gel is: the present invention obtains described ultra-high salt supported hydrogel by polyreaction after preparing the aqueous solution of required salts solution, organic monomer and linking agent mixed solution, initiator, one-step polymerization method makes described gel, success together is stored in salt and water in the high-molecular gel network structure, has realized water, the integrated regulation and control of salt.
The present invention selects linking agent kind, consumption, select suitable function monomer to regulate the functional structure of gel, when being applied to prepare the gel state fertilizer of chemical fertilizer and water integrated controlled release, soluble salt is present in the hydrogel with molecule or ionic form, based on infiltration diffusion principle, their sustainable supply plant moistures and nutritive ingredient nitrogen, phosphorus and potassium and other plant desired nutritional element.Utilize the sustained release of the functional structure of gel, improve utilization rate of fertilizer, reduce the amount of application of chemical fertilizer, reduce the pollution of chemical fertilizer environment to inclusion.The production of described ultra-high salt supported hydrogel and using conveniently, preserve moisture and fertility is effective, and general water-holding agent of cost and controlled release are loose for reducing.At aspects such as horticultural gardening, keeping crop seedling from drought and desert transformations good application prospects will be arranged.
Beneficial effect of the present invention is summarized as follows:
1. raw materials such as salt (solvable chemical fertilizer), organic monomer, linking agent and initiator obtain easily, and single stage method makes gel state fertilizer, and technology is simple, easily control;
2. nutritive substance chemical fertilizer and moisture that plant-growth is required together are stored in the high-molecular gel network structure, have broken through the simple function of traditional water-holding agent water conservation, realize water, fertile integrated regulation and control;
3. the ultra-high salt supported hydrogel stable performance that makes by method of the present invention, but prolonged preservation.
4. nutriment in a fertilizer in the ultra-high salt supported hydrogel and moisture, nationality infiltration diffusion principle sustainable supply crop alimentary, this has been widely used at aspects such as horticultural gardening, keeping crop seedling from drought, desert treatments.
Embodiment
Further describe the present invention below in conjunction with specific embodiment.It below only is several embodiments of the present invention, technical scheme of the present invention is to obtain through secular, a large amount of experimental summaries, this area technological method general, conventional use comprises the control of temperature control, inert atmosphere, the combination and alternative can not the giving unnecessary details one by one in an embodiment of functional similarity material, but does not therefore limit scope of the present invention.
Embodiment 1
(1) prepares the aqueous solution of concentration 50% with ammonium nitrate;
(2) use in the sodium hydroxide and vinylformic acid, the degree of neutralization of carboxyl is 70%;
With the organic monomer acrylamide and and the vinylformic acid of carboxyl and the amount of substance mixed that linking agent α-Jia Jibingxisuan glycidyl ester, methylene-bisacrylamide are pressed 1.5:3:0.2:0.3, join while stirring in the described aqueous ammonium nitrate solution of step (1), the weight percentage of organic monomer and linking agent is 3%.Use the nitrogen protection polymerization system, 75 ℃ of control solution temperatures;
(3) ammonium persulfate solution of weight percentage 10% is under agitation joined in the solution that step (2) makes; the add-on of ammonium persulphate is 1% of an organic monomer total mass; use the nitrogen protection polymerization system; 75 ℃ of control solution temperatures; polyreaction 3 hours promptly gets the hydrogel of superelevation ammonium nitrate load.
The beneficial effect of present embodiment is: superelevation ammonium nitrate load gel state fertilizer has ammonium nitrate content height, ammonium nitrate and water integrated, stable storing, uses characteristics easily.
Embodiment 2
(1) preparing concentration with ammonium chloride is 30% the aqueous solution;
(2) use in the ammonium hydroxide and the carboxyl of α-Jia Jibingxisuan, the degree of neutralization of carboxyl is 100%;
With organic monomer acrylamide, Propylene glycol monoacrylate and and the α-Jia Jibingxisuan of carboxyl and the amount of substance mixed that the linking agent methylene-bisacrylamide is pressed 1.5:1:1:0.5, join while stirring in the aqueous ammonium chloride solution, the weight percentage that makes organic monomer and linking agent is 10%.With nitrogen (or argon gas or carbonic acid gas) protection polymerization system, 20 ℃ of control solution temperatures;
(3) Potassium Persulphate, the sodium sulfite solution of weight percentage 15% under agitation joined in the solution that step (2) makes, the add-on of Potassium Persulphate, S-WAT is 0.5% of an organic monomer total mass, polyreaction 2 hours promptly gets the hydrogel of superelevation ammonium chloride load.
The beneficial effect of present embodiment is: superelevation ammonium chloride supported hydrogel has ammonium chloride content height, ammonium chloride and water integrated, stable storing, uses characteristics easily.
Embodiment 3
(1) prepares the mixed aqueous solution of concentration 25% with bicarbonate of ammonia, primary ammonium phosphate;
(2) use in the sodium hydroxide and vinylformic acid, degree of neutralization is 50%;
With organic monomer in and vinylformic acid, acrylamide, α-Jia Jibingxisuan hydroxypropyl acrylate and the linking agent ethylenebis acrylamide of the carboxyl mixed of pressing the amount of substance of 3:1:0.5:0.8, join while stirring in the ammonium salt aqueous solution, making the total weight percentage of organic monomer and linking agent is 10%.Use the nitrogen protection polymerization system, 70 ℃ of control solution temperatures.
(3) the ammonium cerous sulfate solution of weight percentage 20% is under agitation joined in the solution that step (2) makes, the ammonium cerous sulfate consumption is 1.5% of an organic monomer total mass, and polyreaction 2 hours promptly gets hydrogel of the present invention.
The beneficial effect of present embodiment is: ultra-high salt supported hydrogel of the present invention contains two kinds of nutritive elements of nitrogen, phosphorus of crop needs, has the characteristics of composite fertilizer, the salts contg height, and salt is water integrated, and stable storing is used conveniently.
Embodiment 4
(1) prepares the mixed-ammonium salt aqueous solution of concentration 45% with ammonium nitrate, Secondary ammonium phosphate;
(2) mixed that organic monomer p-sulfonic acid vinylbenzene, Hydroxyethyl acrylate, acrylamide and linking agent α-Jia Jibingxisuan glycidyl ester are pressed the amount of substance of 0.5:1:2.5:0.8, join while stirring in the ammonium salt aqueous solution, the weight percentage that makes organic monomer and linking agent is 5%.Use the nitrogen protection polymerization system, 30 ℃ of control solution temperatures;
(3) hydrogen peroxide, the copperas solution of weight percentage 25% under agitation joined in the solution that step (2) makes, the add-on of hydrogen peroxide, ferrous sulfate is 0.8% of an organic monomer total mass, polyreaction 4 hours promptly gets ultra-high salt supported hydrogel of the present invention.
The beneficial effect of present embodiment is: ultra-high salt supported hydrogel of the present invention contains two kinds of nutritive elements of nitrogen, phosphorus of crop needs, and single stage method is polymerized.Described hydrogel has the characteristics of composite fertilizer, and the salts contg height, and stable storing is used conveniently.
Claims (10)
1, a kind of preparation method of ultra-high salt supported hydrogel is characterized in that being one-step polymerization method, may further comprise the steps:
(1) with the water-soluble preparation salts solution of soluble salt;
(2) with in organic monomer and the salts solution that joins step (1) preparation after linking agent mixes, make and treat polymeric solution; And adopt inert atmosphere protection to treat polymerization system, hierarchy of control temperature;
(3) initiator is made the aqueous solution, what join that step (2) makes treats that in the polymeric solution, polyreaction obtains ultra-high salt supported hydrogel.
2,, it is characterized in that the described inert atmosphere of step (2) is any one or the multiple gases atmosphere in nitrogen, argon gas or the carbonic acid gas according to the preparation method of the described ultra-high salt supported hydrogel of claim 1; Hierarchy of control temperature is 10～90 ℃.
3,, it is characterized in that described organic monomer of step (2) and the linking agent mass percent in the described salts solution of step (1) is 1～20% according to the preparation method of the described ultra-high salt supported hydrogel of claim 1; Linking agent is 1:10～1:5 with the ratio of the amount of organic monomer.
4,, it is characterized in that described organic monomer is any one or a two or more mixture of vinylformic acid, α-Jia Jibingxisuan, acrylamide, vinylbenzene, alpha-methyl styrene, vinyl acetate between to for plastic, p-sulfonic acid vinylbenzene, Hydroxyethyl acrylate, α-Jia Jibingxisuan hydroxyl ethyl ester, Propylene glycol monoacrylate or α-Jia Jibingxisuan hydroxypropyl acrylate according to the preparation method of claim 1 or 3 described ultra-high salt supported hydrogels.
5,, it is characterized in that described linking agent is any one or a two or more mixture of ethylene glycol diacrylate, glycol methacrylate, methylene-bisacrylamide, ethylenebis acrylamide, glycidyl acrylate or α-Jia Jibingxisuan glycidyl ester according to the preparation method of claim 1 or 3 described ultra-high salt supported hydrogels.
6,, it is characterized in that the initiator weight percentage is 5～30% in the aqueous solution of the described initiator of step (3) according to the preparation method of the described ultra-high salt supported hydrogel of claim 1; The consumption of initiator is controlled to be 0.5～5% of organic monomer total mass.
7,, it is characterized in that described initiator is one or more the mixture in ceric sulfate, hydrogen peroxide, ammonium persulphate, Potassium Persulphate, ammonium cerous sulfate, ferrous sulfate, sodium bisulfite or the S-WAT according to the preparation method of the described ultra-high salt supported hydrogel of claim 6.
8,, it is characterized in that the described polymerization reaction time of step (3) is 0.5～5 hour according to the preparation method of the described ultra-high salt supported hydrogel of claim 1.
9, the preparation method's of the described ultra-high salt supported hydrogel of a kind of claim 1 application is characterized in that being applied to prepare salt and water integrated controlled release preparation.
10,, it is characterized in that being applied to prepare the gel state fertilizer of chemical fertilizer and water integrated controlled release according to the preparation method's of the described ultra-high salt supported hydrogel of claim 9 application.
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| CNA2008102194010A CN101429077A (en) | 2008-11-25 | 2008-11-25 | Process for producing ultra-high salt supported hydrogel |
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| CNA2008102194010A CN101429077A (en) | 2008-11-25 | 2008-11-25 | Process for producing ultra-high salt supported hydrogel |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104446846A (en) * | 2013-09-12 | 2015-03-25 | 仲恺农业工程学院 | Water -absorbing water-retention slow and controlled release fertilizer preparation method |
| CN109810225A (en) * | 2019-03-13 | 2019-05-28 | 同济大学 | A kind of crystal type composite gel electrolyte and its preparation method and application |
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2008
- 2008-11-25 CN CNA2008102194010A patent/CN101429077A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104446846A (en) * | 2013-09-12 | 2015-03-25 | 仲恺农业工程学院 | Water -absorbing water-retention slow and controlled release fertilizer preparation method |
| CN109810225A (en) * | 2019-03-13 | 2019-05-28 | 同济大学 | A kind of crystal type composite gel electrolyte and its preparation method and application |
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Application publication date: 20090513 |