CN103159895A - Preparation method of biodegradable and farm-oriented water-absorbing adhesive resin - Google Patents
Preparation method of biodegradable and farm-oriented water-absorbing adhesive resin Download PDFInfo
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- CN103159895A CN103159895A CN2011104219974A CN201110421997A CN103159895A CN 103159895 A CN103159895 A CN 103159895A CN 2011104219974 A CN2011104219974 A CN 2011104219974A CN 201110421997 A CN201110421997 A CN 201110421997A CN 103159895 A CN103159895 A CN 103159895A
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Abstract
The invention discloses a biodegradable and farm-oriented water-absorbing adhesive resin which is prepared by the following raw materials by mass ratio: 75-160 parts of starch, 80-150 parts of acrylic acid, 250-500 parts of a 1 % hydrochloric acid solution, 125-250 parts of a 1 % sulfuric acid solution, 20-70 parts of sodium hydroxide, 1.50-12.00 parts of an initiator: persulfate, 0.75-6.00 parts of bisulfate, 2-6 parts of urea, 0.4-4.0 parts of a cross-linking agent: N, N-methylene-bis-acrylamide, and 0.4-4 parts of borax. The resin is low in cost and good in biodegradability, and has performances of large water-absorbing capacity and viscosity, with a water absorbency being 70-247 times and the viscosity being 0.165 ~ 4.200 Pa*s. The invention further discloses a preparation method of the biodegradable and farm-oriented water-absorbing adhesive resin.
Description
Technical field
The invention belongs to the biodegradable polymer field, particularly a kind of Biodegradable agricultural suction binding resin and preparation method thereof.
Background technology
In recent years, the loss of a large amount of fertilizer NPK that the famine of water resources and soil erosion cause, become the significant problem that the agricultural industry needs to be resolved hurrily, countries in the world are to all very the concerns of the sustainable development of agricultural, all in the development and application dynamics that strengthens bio-organic fertilizer, improve the utilization ratio of fertilizer nutrient NPK, so how to improve the utilization ratio of limited water resources and the great attention that fertilizer nutrient slowly-releasing rate is subject to Chinese scholars in farmland soil always.For the NPK utilization ratio, control widespread pollution from the overuse of fertilizers and pesticides in rural area, promotion agricultural and the ecological Sustainable development that improve fertilizer, countries in the world begin to research and develop coated slow release fertilizer one after another, and this class slow release fertilizer mainly is comprised of NPK nutrient, fertilizer binding agent and coated fertilizer.High hydrophilous resin is as a kind of functional high molecule material, because it has very high water-absorbent and water-retentivity, but the hydrogel slow/controlled release after suction is put in a suitable place to breed minute and moisture utilizes for crop, water-absorbing resin can strengthen water retention, improve Soil structure, reduce the loss of soil moisture and nutrient NPK, be used as the preparation that a kind of coated fertilizer is widely used in slow release fertilizer.In the production process of slow release fertilizer, binding agent is the key factor of fertilizer granulating, and the kind of binding agent and content all affect intensity and the size of slow-release fertilizer granulating, and slow release effect.
The research key of film-coated and slow release fertilizer is degradability and the cheapness of its coated fertilizer and matrix material, can move towards the land for growing field crops.At present a lot of as the kind that raw material prepares High hydrophilous resin and binding agent with the modification of natural reproducible product, method is also varied, but their function singleness only has the function of coating or bonding.The present invention is incorporated into the function of water-absorbing resin and binding agent among a kind of material, has increased the practicality of material.The present invention is with natural macromolecular material cheapness, reproducible, as starch, rice bran etc. for raw material by oxidation, grafting, the method such as crosslinked, adopt water solution polymerization process to prepare a kind of degradable agricultural bonding water-absorbing material, this kind material is on the one hand as binding agent, the process that is prepared into particle at fertilizer plays crucial effect, with having certain water-absorbent after its oven dry, played the function of solid water water conservation simultaneously.This kind material is applied to the preparation of slow-release fertilizer, at first, compare on production technique in traditional technology, granulation and coating one step process are completed, can make Water-retaining slow-release fertilizer; Secondly, the use of new preparation process makes the usage quantity of bonding and coated fertilizer reduce greatly than traditional preparation technology, thereby has reduced greatly the slow-release fertilizer production cost, and water conservation and the large function of slowly/controlled releasing fertilizer nutrient two are arranged.
Summary of the invention
The object of the present invention is to provide a kind of novel degradable agricultural suction binding resin.This resin has good biodegradability, has the characteristics of water-absorbent, cohesiveness and low production cost.
Another object of the present invention is to provide a kind of preparation method of above-mentioned degradable agricultural suction binding resin.The method green non-pollution, production technique is simple.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of Biodegradable agricultural suction binding resin is prepared into by the main raw material of following quality proportioning:
Starch: 75 ~ 160 parts
Vinylformic acid: 80～150 parts
1% hydrochloric acid soln: 250～500 parts, 1% sulphuric acid soln: 125～250 parts
Sodium hydroxide: 20～70 parts
Initiator: persulphate: 1.5～12 parts, hydrosulphite: 0.75～6 part, ceric ammonium nitrate: one or more in 3 ~ 15 parts of three kinds of initiators
Urea: 2～6 parts
Linking agent: N,N methylene bis acrylamide: 0.4～4.0 part, borax: at least a in 0.4～4.0 part
The preparation method of Biodegradable agricultural suction binding resin, key step:
(1) activation: starch is mixed with activated solution, in 60～90 ℃ of activation 0.5～2 hour, then be cooled to below 30 ℃ or 30 ℃;
(2) in and vinylformic acid: sodium hydroxide is soluble in water, add vinylformic acid to carry out neutralization reaction in ice-water bath;
(3) polyreaction: under whipped state, add urea reaction 10～30min of 2～6% in solution after above-mentioned (1) step activate and lower the temperature, then add initiator, above-mentioned (2) vinylformic acid neutralization reaction liquid, the linking agent in going on foot to react 2～5 hours in 50～70 ℃;
(4) be Biodegradable agricultural binding resin of the present invention after the product that (3) is gone on foot is cooling, the product oven dry with (3) step is Biodegradable agricultural water-absorbing resin of the present invention after pulverizing.
It is raw material that Biodegradable agricultural suction binding resin of the present invention adopts extensively cheap starch, through processing the appropriate vinylformic acid of graft copolymerization, be prepared into the resin with suction and the two large functions that bond, its water absorbent rate can reach 70 ~ 247 times, and viscosity can reach 0.165 ~ 4.200 Pas.Compared with prior art, beneficial effect of the present invention is: 1) the preparation slowly/controlled releasing fertilizer on because this material has the function of water conservation and slowly-releasing, make slow release fertilizer have water retaining function, reduced use cost.2) on the preparation technology of slow release fertilizer, with granulation and a synthetic step of coating two step process, reduced production unit and energy consumption, reduce simultaneously the use of matrix material, thereby greatly reduced the production cost of slow-release fertilizer.3) provide a kind of new slow-release fertilizer functional materials, and synthetic method, and the development of promotion slow-release fertilizer technology of preparing.
Embodiment
The present invention is described in further detail below in conjunction with embodiment.But this should be interpreted as that the scope of the above-mentioned theme of the present invention only limits to following embodiment.
Example 1
W-Gum: 5.0g
Vinylformic acid: 3.0g
Sodium hydroxide: 1.25g
Initiator: ammonium persulphate: 0.12g
Linking agent: N,N methylene bis acrylamide: 0.01g.
Above-mentioned degradable agricultural bonding water-absorbing resin, adopt to comprise that the method for following key step makes:
(1) activation: 5g starch is mixed with 25ml water, in 80 ℃ of activation 0.5 hour, then be cooled to 30 ℃;
(2) in and vinylformic acid: in the water-soluble 12ml of sodium hydroxide 1.25g, add vinylformic acid 3g to carry out neutralization reaction in ice-water bath;
(3) polyreaction: under whipped state, add initiator ammonium persulfate 0.12g, the vinylformic acid neutralization reaction liquid in above-mentioned (2) step, N,N methylene bis acrylamide: 0.01g in 70 ℃ of reactions 3 hours in solution after above-mentioned (1) step activates and lowers the temperature;
(4) be Biodegradable agricultural binding resin of the present invention after the product that (3) is gone on foot is cooling, viscosity is measured as 0.165Pas with rotational viscosimeter.Product oven dry with (3) step is Biodegradable agricultural water-absorbing resin of the present invention after pulverizing, water absorbent rate is about 70 times.
Example 2
W-Gum: 5.0g
Vinylformic acid: 5.0g
Sodium hydroxide: 2.08g
Initiator: ammonium persulphate: 0.15g
Linking agent: borax: 0.04g.
Above-mentioned degradable agricultural bonding water-absorbing resin, adopt to comprise that the method for following key step makes:
(1) activation: 5g starch is mixed with 25ml water, in 80 ℃ of activation 1 hour, then be cooled to below 30 ℃ or 30 ℃;
(2) in and vinylformic acid: in the water-soluble 20ml of sodium hydroxide 2.08g, add vinylformic acid 5g to carry out neutralization reaction in ice-water bath;
(3) polyreaction: under whipped state, add initiator ammonium persulfate 0.15g, the vinylformic acid neutralization reaction liquid in above-mentioned (2) step, linking agent borax 0.04g in 60 ℃ of reactions 3 hours in the solution after above-mentioned (1) step activates and lowers the temperature;
(4) be Biodegradable agricultural binding resin of the present invention after the product that (3) is gone on foot is cooling, viscosity is measured as 2.860Pas with rotational viscosimeter.Product oven dry with (3) step is Biodegradable agricultural water-absorbing resin of the present invention after pulverizing, water absorbent rate is about 163 times.
Example 3
W-Gum: 5.0g
Vinylformic acid: 5.0g
1% sulphuric acid soln: 25ml
Sodium hydroxide: 1.94g
Initiator: ammonium persulphate: 0.12g sodium bisulfite: 0.06g
Linking agent: N,N methylene bis acrylamide: 0.02g.
Above-mentioned degradable agricultural bonding water-absorbing resin, adopt to comprise that the method for following key step makes:
(5) activation: 5g starch is mixed with the 25ml1% sulphuric acid soln, in 80 ℃ of activation 0.5 hour, then be cooled to below 30 ℃ or 30 ℃;
(6) in and vinylformic acid: in the water-soluble 20ml of sodium hydroxide 1.94g, add vinylformic acid 5g to carry out neutralization reaction in ice-water bath;
(7) polyreaction: under whipped state, add initiator ammonium persulfate 0.12g, the vinylformic acid neutralization reaction liquid in above-mentioned (2) step, linking agent N,N methylene bis acrylamide 0.02g in 60 ℃ of reactions 3 hours in solution after above-mentioned (1) step activates and lowers the temperature;
(8) be Biodegradable agricultural binding resin of the present invention after the product that (3) is gone on foot is cooling, viscosity is measured as 3.610Pas with rotational viscosimeter.Product oven dry with (3) step is Biodegradable agricultural water-absorbing resin of the present invention after pulverizing, water absorbent rate is about 142 times.
Example 4
W-Gum: 5.0g
Vinylformic acid: 5.0g
1% hydrochloric acid soln: 25ml
Sodium hydroxide: 2.08g
Initiator: ammonium persulphate: 0.12g
1% urea soln: 0.3ml
Linking agent: N,N methylene bis acrylamide: 0.02g.
Above-mentioned degradable agricultural bonding water-absorbing resin, adopt to comprise that the method for following key step makes:
(1) activation: 5g starch is mixed with the 25ml1% hydrochloric acid soln, in 80 ℃ of activation 0.5 hour, then be cooled to below 30 ℃ or 30 ℃;
(2) in and vinylformic acid: in the water-soluble 20ml of sodium hydroxide 2.08g, add vinylformic acid 5g to carry out neutralization reaction in ice-water bath;
(3 polyreactions: under whipped state, the urea reaction 10min that adds 0.3ml in solution after above-mentioned (1) step activates and lowers the temperature, then add initiator ammonium persulfate 0.12g, the vinylformic acid neutralization reaction liquid in above-mentioned (2) step, linking agent N,N methylene bis acrylamide 0.02g in 70 ℃ of reactions 3 hours;
(4) be Biodegradable agricultural binding resin of the present invention after the product that (3) is gone on foot is cooling, viscosity is measured as 4.200Pas with rotational viscosimeter.Product oven dry with (3) step is Biodegradable agricultural water-absorbing resin of the present invention after pulverizing, water absorbent rate is about 247 times.
Claims (7)
1. Biodegradable agricultural suction binding resin is prepared into by the main raw material of following quality proportioning:
Starch: 75 ~ 160 parts
Vinylformic acid: 80～150 parts
1% hydrochloric acid soln: 250～500 parts, 1% sulphuric acid soln: wherein a kind of in 125～250 parts two kinds
Sodium hydroxide: 20～70 parts
Initiator: persulphate: 1.5～12 parts, hydrosulphite: 0.75～6 part, ceric ammonium nitrate: one or more in 3 ~ 15 parts of three kinds of initiators
Urea: 2～6 parts
Linking agent: N,N methylene bis acrylamide: 0.4～4.0 part, borax: at least a in 0.4～4.0 part.
2. Biodegradable agricultural described according to claims 1 suction binding resin is characterized in that:
Described raw material adopts starch and acrylic acid ratio greater than 0.5.
3. Biodegradable agricultural described according to claims 1 suction binding resin is characterized in that:
Described initiator adopts 3 ~ 15 parts of persulphates, hydrosulphite, ceric ammonium nitrate, in three kinds of initiators one or more.
4. Biodegradable agricultural described according to claims 1 suction binding resin is characterized in that:
Described linking agent adopts in N,N methylene bis acrylamide, borax at least a.
5. Biodegradable agricultural described according to claims 1 suction binding resin is characterized in that:
Described raw material has adopted urea.
6. the preparation method of Biodegradable agricultural described according to claims 1 suction binding resin comprises following key step:
1) activation: starch is mixed with activated solution, in 60～90 ℃ of activation 0.5～2 hour, then be cooled to below 30 ℃ or 30 ℃;
2) in and vinylformic acid: sodium hydroxide is soluble in water, add vinylformic acid to carry out neutralization reaction in ice-water bath;
3) polyreaction: under whipped state, add urea reaction 10～30min of 2～6% in solution after above-mentioned (1) step activate and lower the temperature, then add initiator, above-mentioned (2) vinylformic acid neutralization reaction liquid, the linking agent in going on foot to react 2～5 hours in 50～70 ℃;
4) product of step 3 is Biodegradable agricultural binding resin of the present invention after cooling, product that will (3) step is dried, and is Biodegradable agricultural water-absorbing resin of the present invention after pulverizing.
7. suction binding resin agricultural according to the biological degradation of claims 1 and 6 described preparations is characterized in that:
Possess suction and the two large functions that bond are arranged.
Priority Applications (1)
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| CN2011104219974A CN103159895A (en) | 2011-12-16 | 2011-12-16 | Preparation method of biodegradable and farm-oriented water-absorbing adhesive resin |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103337656A (en) * | 2013-07-05 | 2013-10-02 | 中国科学院青岛生物能源与过程研究所 | Modified biomass lithium ion battery adhesive |
| CN103739783A (en) * | 2013-12-27 | 2014-04-23 | 福建农林大学 | Starch water-retaining agent and preparation method thereof |
| 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 |
| CN104030838A (en) * | 2014-06-30 | 2014-09-10 | 成都新柯力化工科技有限公司 | Polymerized sustained-release compound fertilizer and preparation method thereof |
| CN104355794A (en) * | 2014-10-20 | 2015-02-18 | 柳州市天姿园艺有限公司 | Slow release urea |
| CN104557343A (en) * | 2015-02-04 | 2015-04-29 | 安徽帝元生物科技有限公司 | Retention urea |
| CN104557342A (en) * | 2015-02-04 | 2015-04-29 | 安徽帝元生物科技有限公司 | Preparation method of retention urea |
| CN104804355A (en) * | 2015-01-19 | 2015-07-29 | 四川师范大学 | Biodegradable agricultural liquid mulching film and preparation method thereof |
| CN105330954A (en) * | 2015-12-14 | 2016-02-17 | 民勤县邦德贸易有限公司 | Weather-proof resin master batch for agricultural plastic mulching film synthesis and preparation method |
| CN108623748A (en) * | 2018-05-24 | 2018-10-09 | 中国农业大学 | A kind of load boron fibre element super absorbent resin and preparation method thereof |
Citations (1)
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| CN101280044A (en) * | 2008-05-29 | 2008-10-08 | 四川师范大学 | Biodegradable agricultural high-absorbent resin and preparation thereof |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101280044A (en) * | 2008-05-29 | 2008-10-08 | 四川师范大学 | Biodegradable agricultural high-absorbent resin and preparation thereof |
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103337656A (en) * | 2013-07-05 | 2013-10-02 | 中国科学院青岛生物能源与过程研究所 | Modified biomass lithium ion battery adhesive |
| CN103337656B (en) * | 2013-07-05 | 2017-03-15 | 中国科学院青岛生物能源与过程研究所 | A kind of modified biomass Li-like ions battery adhesive |
| CN103739783B (en) * | 2013-12-27 | 2016-01-06 | 福建农林大学 | A kind of starch water-holding agent and preparation method thereof |
| CN103739783A (en) * | 2013-12-27 | 2014-04-23 | 福建农林大学 | Starch water-retaining agent and preparation method thereof |
| 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 |
| CN104030838A (en) * | 2014-06-30 | 2014-09-10 | 成都新柯力化工科技有限公司 | Polymerized sustained-release compound fertilizer and preparation method thereof |
| CN104355794A (en) * | 2014-10-20 | 2015-02-18 | 柳州市天姿园艺有限公司 | Slow release urea |
| CN104804355A (en) * | 2015-01-19 | 2015-07-29 | 四川师范大学 | Biodegradable agricultural liquid mulching film and preparation method thereof |
| CN104557342A (en) * | 2015-02-04 | 2015-04-29 | 安徽帝元生物科技有限公司 | Preparation method of retention urea |
| CN104557343B (en) * | 2015-02-04 | 2017-07-11 | 安徽帝元生物科技有限公司 | A kind of retentivity urea |
| CN104557342B (en) * | 2015-02-04 | 2017-08-29 | 安徽帝元生物科技有限公司 | A kind of preparation method of retentivity urea |
| CN104557343A (en) * | 2015-02-04 | 2015-04-29 | 安徽帝元生物科技有限公司 | Retention urea |
| CN105330954A (en) * | 2015-12-14 | 2016-02-17 | 民勤县邦德贸易有限公司 | Weather-proof resin master batch for agricultural plastic mulching film synthesis and preparation method |
| CN108623748A (en) * | 2018-05-24 | 2018-10-09 | 中国农业大学 | A kind of load boron fibre element super absorbent resin and preparation method thereof |
| CN108623748B (en) * | 2018-05-24 | 2020-06-12 | 中国农业大学 | Boron-loaded cellulose super absorbent resin and preparation method thereof |
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Application publication date: 20130619 |