CN101353283A - Preparation of acrylic ester mixed polymer urea slow release coating agent - Google Patents
Preparation of acrylic ester mixed polymer urea slow release coating agent Download PDFInfo
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- CN101353283A CN101353283A CNA2008102220509A CN200810222050A CN101353283A CN 101353283 A CN101353283 A CN 101353283A CN A2008102220509 A CNA2008102220509 A CN A2008102220509A CN 200810222050 A CN200810222050 A CN 200810222050A CN 101353283 A CN101353283 A CN 101353283A
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Abstract
The invention discloses a preparation method of a urea slow-release film coating agent of an acrylic ester mixed polymer, which comprises the following steps: the preparation of the acrylic ester mixed polymer, the preparation of water-soluble polymer water solution and the preparation of the slow-release film coating agent of the acrylic ester mixed polymer. The preparation method takes water as a polymerization medium, polymer emulsion prepared by segmentation emulsion polymerization effectively controls water resistance and mechanical properties of slow-release materials, and the polymer emulsion is added with the water-soluble polymer material to improve the film forming capacity of the emulsion and the stability of the film material. The method has the advantages that no organic solvent is adopted during the production process, no waste gas and waste liquid is produced, and the slow-release film coating material obtained has good film forming effect, excellent slow-release function and good water solubility, therefore, the slow-release film coating agent is an ideal environment-friendly film coating material.
Description
Technical field
The present invention relates to the preparation method of a kind of fertilizer slow release coating agent, be specifically related to a kind of preparation method of acrylic ester mixed polymer urea slow release coating agent.
Background technology
The principal item of nitrogenous fertilizer is urea both at home and abroad, is to use maximum nitrogen fertilizers in the world, and in most of areas, in torrid areas, arid or semiarid zone and paddy field, the fertilizer efficiency of urea seldom surpasses 50%.The one of the main reasons of urea fertilizer loss, it is urea hydrolysis rapidly under the katalysis of soil urease, thereby the volatilization loss that causes ammonia, in order to improve the utilization ratio of nitrogen in the urea, the U.S., Japan, European Union adopt resin or sulphur coated urea, and domestic production enterprise has introduced the coated with resin technology, though can play the effect of control fertilizer efficiency slowly-releasing to a certain extent, but resin is difficult to degraded in soil, long-term application will be destroyed Soil structure.At present, China's crop species is various, need different sorts, different time sections to discharge the coated slow release formulation of nutrient, exist contaminate environment with thermoplastic resin as the coated slow-release material, shortcomings such as solvent is toxic are needed a kind of coated fertilizer that all compares environmental protection in production still is use of exploitation badly.
Summary of the invention
The objective of the invention is to provide a kind of preparation method of acrylic ester mixed polymer urea slow release coating agent at the deficiencies in the prior art.It is to utilize emulsion polymerization technology, adds the water tolerance of vinylbenzene with the raising mould material in polymerization process, adds the elasticity that cross-linking monomer improves rete, adopts segmentation to mix the water tolerance and the mechanical property of poly-next effective controlling slow release material simultaneously.Add film forming properties and the film material stability that water-soluble high-molecular material improves emulsion in emulsion, make the coated slow-release material possess good film-formation result and excellent slow control-release function, be 100-120 days the time of releasing of blood urea nitrogen in soil.Simultaneously, make such material coated slow release urea can be suitable for food crop, be applicable to solanaceous vegetables again by the prescription that changes coated fertilizer.
The technology used in the present invention principle:
(1) adopt substep letex polymerization way, after water soluble starter decomposed the generation free radical at a certain temperature, the acrylic acid or the like function monomer was through forming stable acrylic ester mixed polymer emulsion after the letex polymerization.
(2) utilize the water resistance and the good film forming properties of polyvinyl alcohol solution of styrol copolymer in the acrylic ester mixed polymer, acrylic ester mixed polymer is mixed by a certain percentage with polyvinyl alcohol water solution, promptly become the agent of urea special slow release coating.
The technical solution adopted in the present invention: a kind of preparation method of acrylic ester mixed polymer urea slow release coating agent comprises the preparation section of acrylic ester mixed polymer, the preparation section of the water-soluble polymer aqueous solution, the preparation section of acrylic ester mixed polymer slow release coating agent.Its concrete steps are as follows:
1, the preparation section of acrylic ester mixed polymer
Reaction system is raw materials used: vinylformic acid, butyl acrylate, methyl methacrylate, vinylbenzene, vinyl cyanide, acrylamide, 92%～93% N hydroxymethyl acrylamide, ammonium persulphate, 25% ammoniacal liquor, wherein the degree of each ingredients constitute raw material total mass is: vinylformic acid 10～14%, butyl acrylate 10～50%, methyl methacrylate 2～15%, vinylbenzene 30～55%, vinyl cyanide 3～5%, acrylamide 3～5%, 92%～93% N hydroxymethyl acrylamide 1～3%, water-soluble persulphate radical polymerization initiator is (as Potassium Persulphate, ammonium persulphate) 0.5～1%, 25% ammoniacal liquor 0.1～5%; In addition, the Virahol consumption is a reaction system total mass 1～10%, and the quality of deionized water is 50～60% of a reaction system total mass, and the anionic emulsifier consumption is 1～4% of a deionized water quality.
Preparation section:
(1), anionic emulsifier is added in the deionized water, in reactor, be stirred to dissolving fully, add acrylamide again, be stirred to dissolving fully, the aqueous solution is heated to 70～80 ℃ then.Described anionic emulsifier is Sodium dodecylbenzene sulfonate or sodium lauryl sulphate.
(2), with vinylformic acid, methymethacrylate, Virahol consumption 10%～50%, 10%～50% the mixing and stir and obtain mixed solution of butyl acrylate consumption, then mixed solution is joined in the reactor, and add the part ammonium persulphate, 70～80 ℃ of following polyreactions 0.7～1.5 hour.
(3), surplus Virahol and butyl acrylate are mixed in the back adding reactor; Half of one half-sum vinyl cyanide consumption of vinylbenzene consumption mixed the back to add in the reactor; And will add the surplus ammonium persulphate, reacted 1～2 hour down at 80～84 ℃.
(4), N hydroxymethyl acrylamide and remaining half vinylbenzene and vinyl cyanide are joined continue reaction 0.5～1 hour in the reactor again.
(5), when the temperature in the reactor is reduced to 50～60 ℃, add 25% ammoniacal liquor and carry out neutralization reaction.
(6) continue stirring and be cooled to 40 ℃ with down to room temperature, be acrylic ester mixed polymer, the discharging barrelling is standby.
2, the preparation section of the water-soluble polymer aqueous solution
Add deionized water in reactor, heating treats that temperature rises to more than 90 ℃, adds water-soluble high-molecular material in proportion, is stirred to fully and is mixed with the 10% water-soluble polymer aqueous solution after the dissolving.Described water-soluble high-molecular material is the mixing of a kind of, two or more arbitrary proportion in natural macromolecular material, semi-synthetic family macromolecule material or the synthetic family macromolecule material.Described natural macromolecular material is starch, sodium alginate, agar-agar, vegetable jelly, gelatin or microbiological gum.Described semi-synthetic family macromolecule material is modified-cellulose or treated starch.Described synthetic family macromolecule material is polyacrylamide, polyvinyl alcohol, polyethylene oxide, polymaleic anhydride, water soluble amino resin, water soluble phenol resin, water soluble alkyd resin, water-soluble epoxy resin, water soluble polyurethane resin or water-soluble poly-sucrose.
3, the preparation section of acrylic ester mixed polymer slow release coating agent
The acrylic ester mixed polymer and the 10% water-soluble polymer aqueous solution are pressed mass ratio 1: 0.2～1: 2, under 80～95 ℃ of conditions, mix, promptly become acrylic ester mixed polymer urea slow release coating agent.
The present invention is polymerisation medium with water, the macromolecule emulsion that utilizes the mode of segmentation letex polymerization to prepare, the water tolerance and the mechanical property of effective controlling slow release material, and in emulsion, add film forming properties and the film material stability that water-soluble high-molecular material improves emulsion, the coated slow-release material for preparing possesses good film-formation result and excellent slow control-release function, there is not organic solvent, there is not waste gas and waste liquid in the production process, having advantages such as good water solubility, is the coated fertilizer of a kind of comparatively ideal environmental protection.
Embodiment
The invention will be further described with indefiniteness embodiment below.
Embodiment,
(1) in polymerization reaction kettle, adds deionized water 300kg, start stirrer.
(2) add Sodium dodecylbenzene sulfonate 6.0kg, to dissolving fully.
(3) stir adding acrylamide 10kg down,, open the low-pressure steam heating to dissolving fully.
(4) add 30kg Virahol and 50kg butyl acrylate in mixing stirred pot, 30kg vinylformic acid and 30kg methymethacrylate mix.When aqueous temperature rises to 75 ℃ of left and right sides in the question response still, above-mentioned mixing solutions is squeezed into reactor with pump, and add the 2kg ammonium persulphate, 80 ℃ of following polyreactions 1 hour.
(5) in mixing stirred pot, add 20kg Virahol and 30kg butyl acrylate, mix the back and squeeze into reactor with pump; In another mixing tank, add 50kg vinylbenzene and 5kg vinyl cyanide, after mixing, squeeze into reactor with pump; And add the 2kg ammonium persulphate, 82 ℃ were reacted 1.5 hours down.
(6) add 6kg N hydroxymethyl acrylamide and remaining 50kg vinylbenzene and 5kg vinyl cyanide, continue reaction 1 hour.
(7) steam off valve starts cooling water circulation cooling.When temperature is reduced to 60 ℃, add 25% ammoniacal liquor, carry out neutralization reaction.
(8) continue stirring and be cooled to 40 ℃, be acrylic ester mixed polymer, the discharging barrelling.
(9) in reactor, add deionized water 300kg, start agitator and low-pressure steam, treat that temperature rises to more than 90 ℃, add polyvinyl alcohol 30kg, promptly become 10% polyvinyl alcohol water solution after the dissolving fully.
(10) acrylic ester mixed polymer and 10% polyvinyl alcohol water solution are pressed mass ratio 1: 0.8, under 80～95 ℃ of conditions, mix, promptly become acrylic ester mixed polymer urea slow release coating agent.
The use of acrylic ester mixed polymer coated slow release formulation
1, in mixing kettle, adds the acrylic ester mixed polymer coated slow release formulation, be heated with stirring to 80 ℃, added the kaolin in 400 mesh sieve holes, stir and make it thorough mixing.
2, start the cylinder encapsulation tool, use travelling belt to add granular urea (particle diameter 3.35～5.6mm) on one side from charging opening, by material lifting flights urea granules is kicked up, using pressurised metered pump that above-mentioned coated slow release formulation is vaporific by nozzle on one side is sprayed on the urea granules, urea is kicked up, is fallen in the fog-zone of coating agent, kicking up falls again again, thereby is wrapped the last layer coated slow release formulation so repeatedly, and the consumption of sustained release dosage is 1%～1.5% of a urea quality.
3, (6～8r/min), the urea granules that is wrapped enters 90～95 ℃ of hot blast districts, rapidly oven dry along with the rotation of coating tube.
4, by travelling belt, the coated carbamide of being dried enters cooling cylinder, rapidly cooling.
5, be delivered into finished bin by travelling belt, adopt the automatic packing machine packing.
The slow release effect of acrylic ester mixed polymer release-controlled coated urea
1, water wash effect
67.16%, 3 cumulative leaching rate 99.06% of the elementary solubility rate of urea;
Coated carbamide: 13.40%, 18 cumulative leaching rate 94.88% of elementary solubility rate.
European Union's resin and sulfur coating urea proposed standard regulation: elementary solubility rate≤15%; The U.S. and Japanese resin coated urea proposed standard regulation: elementary solubility rate≤40%; Japan's fertilizer law (1996) is stipulated elementary nitrogen solubility rate＜50% to field crop.From the water wash result, the effect of acrylic ester mixed polymer sustained release dosage coated carbamide still is good.
2, field crops fertilizer efficiency
2.1. test soil
Changping, Beijing " national brown moisture soil scholar earth fertility and fertilizer benefit monitoring base ", the moisture soil great soil group, brown moisture soil penus, the soil texture is a silt loam.Soil physical and chemical property: pH value 8.11, organic 16.42gkg
-1, full nitrogen (N) 0.893gkg
-1, rapid available phosphorus (P
2O
5) 9.79mgkg
-1, available potassium (K
2O) 40mgkg
-1Wheat breed: capital 9428; Corn variety: middle list 8578.
2.2. test method
3 processing are established in test altogether, 3 repetitions.Sub-district area: 10m
2(2.5m * 4m), rate of fertilizer application: N180kg/hm
2Season, phosphorus (P
2O
5) kg/hm
2Season, potassium (K
2O) 96kg/hm
2Season.Handle 1, space management CK (not applying fertilizer); Handle 2, conventional fertilizer application; Handle 3, coated carbamide.Processing 2 and processing 3 equivalent are used.
2.3. wheat and corn test-results
Table 1 different treatment sugarcane yield result
Annotate: " * * " expression difference reaches utmost point conspicuous level in the table
As can be seen from Table 1, use under the NPK condition in equivalent, coated carbamide is handled ratio and is waited NPK to handle output increase 86.6kg/667m
2, volume increase 17.2% through variance analysis, is used nitrogen amount urea such as coated carbamide and use and is compared with not applying fertilizer, and volume variance all reaches utmost point conspicuous level.。
3, field crops fertilizer efficiency
3.1. test site and confession examination material
Test is carried out in orchid ocean, Bai Majing town, Danzhou, Hainan, and the soil texture is middle earth, soil physical and chemical property: pH value 5.11, organic 9.7gkg
-1, full nitrogen (N) 0.651gkg
-1, rapid available phosphorus (P
2O
5) 9.10mgkg
-1, available potassium (K
2O) 34.0mgkg
-1Sugar cane breed: Guangdong sugar 93/159.
3.2. test method
3 processing are established in test altogether, 3 repetitions.Sub-district area: 18m
2(5m * 3m), rate of fertilizer application: N450kg/hm
2, phosphorus (P
2O
5) 300kg/hm
2, potassium (K
2O) 500kg/hm
2Handle 1, space management CK (not applying fertilizer); Handle 2, conventional fertilizer application; Handle 3, coated carbamide.Processing 2 and processing 3 nutrients such as grade are used.
3.3. test-results
Table 2 different treatment sugarcane yield result
Annotate: " * * " expression difference reaches utmost point conspicuous level in the table
Table 2 as can be seen, different treatment is very big to sugarcane yield influence, handles 3 and improves 4430kg/667m than handling 1 output
2, volume increase 126.6%.Handle 3 than handling 2 increase 1480kg/667m
2, volume increase 22.9%.Through variance analysis, to use coated carbamide and compare with not applying fertilizer with nitrogen amount urea such as uses, volume variance all reaches utmost point conspicuous level.
Claims (5)
1, a kind of preparation method of acrylic ester mixed polymer urea slow release coating agent is characterized in that: comprise the preparation section of acrylic ester mixed polymer, the preparation section of the water-soluble polymer aqueous solution, the preparation section of acrylic ester mixed polymer slow release coating agent; Its concrete steps are as follows:
1), the preparation section of acrylic ester mixed polymer
Reaction system is raw materials used: vinylformic acid, butyl acrylate, methyl methacrylate, vinylbenzene, vinyl cyanide, acrylamide, N hydroxymethyl acrylamide, water-soluble persulphate radical polymerization initiator is (as Potassium Persulphate, ammonium persulphate), ammoniacal liquor, wherein the degree of each ingredients constitute raw material total mass is: vinylformic acid 10～14%, butyl acrylate 10～50%, methyl methacrylate 2～15%, vinylbenzene 30～55%, vinyl cyanide 3～5%, acrylamide 3～5%, 92%～93% N hydroxymethyl acrylamide 1～3%, water-soluble persulphate radical polymerization initiator is (as Potassium Persulphate, ammonium persulphate) 0.5～1%, 25% ammoniacal liquor 0.1～5%; In addition, the Virahol consumption is a reaction system total mass 1～10%, and the quality of deionized water is 50～60% of a reaction system total mass, and the anionic emulsifier consumption is 1～4% of a deionized water quality;
Preparation section:
(1), anionic emulsifier is added in the deionized water, in reactor, be stirred to dissolving fully, add acrylamide again, be stirred to dissolving fully, the aqueous solution is heated to 70～80 ℃ then.Described anionic emulsifier is Sodium dodecylbenzene sulfonate or sodium lauryl sulphate;
(2), with vinylformic acid, methymethacrylate, Virahol consumption 10%～50%, 10%～50% the mixing and stir and obtain mixed solution of butyl acrylate consumption, then mixed solution is joined in the reactor, and add the part ammonium persulphate, 70～80 ℃ of following polyreactions 0.7～1.5 hour;
(3), surplus Virahol and butyl acrylate are mixed in the back adding reactor; Half of one half-sum vinyl cyanide consumption of vinylbenzene consumption mixed the back to add in the reactor; And will add the surplus ammonium persulphate, reacted 1～2 hour down at 80～84 ℃;
(4), N hydroxymethyl acrylamide and remaining half vinylbenzene and vinyl cyanide are joined continue reaction 0.5～1 hour in the reactor again;
(5), the temperature in the reactor is reduced to 50～60 ℃, add 25% ammoniacal liquor and carry out neutralization reaction;
(6) continue stirring and be cooled to 40 ℃ with down to room temperature, be acrylic ester mixed polymer, the discharging barrelling is standby;
2), the preparation section of the water-soluble polymer aqueous solution
Add deionized water in reactor, heating treats that temperature rises to more than 90 ℃, adds water-soluble high-molecular material in proportion, is stirred to fully and is mixed with the 10% water-soluble polymer aqueous solution after the dissolving;
3), the preparation section of acrylic ester mixed polymer slow release coating agent
The acrylic ester mixed polymer and the 10% water-soluble polymer aqueous solution are pressed mass ratio 1: 0.2～1: 2, under 80～95 ℃ of conditions, mix, promptly become acrylic ester mixed polymer urea slow release coating agent.
2, the preparation method of acrylic ester mixed polymer urea slow release coating agent according to claim 1 is characterized in that: described water-soluble high-molecular material is the mixing of a kind of, two or more arbitrary proportion in natural macromolecular material, semi-synthetic family macromolecule material or the synthetic family macromolecule material.
3, the preparation method of acrylic ester mixed polymer urea slow release coating agent according to claim 2 is characterized in that: described natural macromolecular material is starch, sodium alginate, agar-agar, vegetable jelly, gelatin or microbiological gum.
4, the preparation method of acrylic ester mixed polymer urea slow release coating agent according to claim 2 is characterized in that: described semi-synthetic family macromolecule material is modified-cellulose or treated starch.
5, the preparation method of acrylic ester mixed polymer urea slow release coating agent according to claim 2 is characterized in that: described synthetic family macromolecule material is polyacrylamide, polyvinyl alcohol, polyethylene oxide, polymaleic anhydride, water soluble amino resin, water soluble phenol resin, water soluble alkyd resin, water-soluble epoxy resin, water soluble polyurethane resin or water-soluble poly-sucrose.
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