CN104829340A - Microcapsule graphene composite material controlled-release pesticide-fertilizer granules and preparation method - Google Patents
Microcapsule graphene composite material controlled-release pesticide-fertilizer granules and preparation method Download PDFInfo
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Abstract
The present invention relates to microcapsule graphene composite material controlled-release pesticide-fertilizer granules, which comprise mother powder, an inorganic nutrient, an organic matter, an anti-hardening agent and a filler, wherein the mother powder comprises a microcapsule graphene composite material and a pesticide active ingredient, the microcapsule graphene composite material is formed by compounding a polymer compound and graphite powder, and the polymer compound is at least one selected from gelatin, gum arabic, starch, chitosan, alginic acid, methyl cellulose, a carboxymethyl cellulose salt, poly lactic acid, polyamide and polyvinyl alcohol. The preparation method comprises: completely mixing pesticide and graphite powder, crushing, placing the obtained mixture and a polymer compound into a ball mill to grind, carrying out agglomeration, precipitation or polymerization to obtain a mixture of the microcapsule graphene composite material and the pesticide, drying to obtain mother powder, carrying out granulation on the mother powder, an inorganic nutrient, an organic matter and a filler, and spraying an anti-hardening agent on the particles so as to obtain the finished product. According to the present invention, the release is stable, and the problems of fertilizer applying and plant diseases and insect pests of the whole season can be solved with the applying of the granules one time.
Description
Technical field
The present invention relates to fertilizer field, be specifically related to the fertile field of organic-inorganic medicine, particularly a kind of controlled release fertilizer granules containing pesticide active ingredient and micro-capsule graphene composite material and preparation method thereof.
Background technology
Medicine fertilizer is generally by medicine and fertile " uniting two into one ", is exactly " the fertile integration of medicine ".Medicine fertilizer has one or more the function in control diseases and pests of agronomic crop or regulating crop growth, and can provide nutrition for farm crop or have the multi-Functional Fertilizers providing nutrition and improve fertilizer and agricultural chemicals utilization ratio simultaneously.There is balance fertilizing, nutrition is complete; Broad-spectrum high efficacy, once to settle; Urge after front control, strengthen resistance; Fertile medicine combines, does synergy mutually; Easy and simple to handle, use safety; Dart transfer, increasing both production and income; Expect with fertile generation, safety and environmental protection; Accumulating is convenient, low-carbon energy-saving; In many ways be benefited, the nine large advantages such as to benefit the nation and the people.The agricultural chemicals used in agricultural and fertilizer two kinds of most important agrochemicals are united by it, two, the nutrient supply field operation of the plant protection of agricultural chemicals and fertilizer are united two into one, and save labour, reduce production cost.When agricultural chemicals and fertilizer are all in the optimal application phase, drug effect and fertilizer efficiency can be improved.
Slow/controlled release medicine fertilizer can improve utilization rate of fertilizer, partly solve cause because of excessive fertilization ecological environment problem, natural resources and energy resources dual waste problem, greatly alleviate the murder by poisoning of high toxicity chemical substance to mammal, greatly extend the lasting period of same dose agricultural chemicals, reduce degraded and its drug wastage caused because of evaporation and liquid-flow of agricultural chemicals, reduce solvent load, reduce labour intensity, be a kind of new and effective fertilizer, there is good development prospect.Now be no lack of on the market slow/controlled release medicine fertilizer occur, but they have slowly-releasing is achieved to fertilizer, what have achieves slowly-releasing to medicine, but be difficult to slowly-releasing is realized to fertilizer and medicine simultaneously, do not reach single-dose application, the object of the medication that do not refertilize in a season.
Summary of the invention
Technical problem to be solved by this invention is the stability that solution fertilizer and agricultural chemicals mix, and realizes the Co ntrolled release of agricultural chemicals and fertilizer, improves the lasting period of agricultural chemicals and fertilizer, reaches or substantially reach the object that a time need not refertilize and spray medicine dispenser whole season.
The present invention solves the problems of the technologies described above taked technical scheme: a kind of micro-capsule graphene composite material controlled release fertilizer granules, is made up of female powder, inorganic nutrients, organic matter, hardening resisting agent and filler;
Described female powder is made up of micro-capsule graphene composite material and pesticide active ingredient;
Described micro-capsule graphene composite material is composited by macromolecular compound and Graphite Powder 99, and described macromolecular compound is at least one in gelatin, gum arabic, starch, chitosan, Lalgine, methylcellulose gum, carboxymethyl cellulose salt, poly(lactic acid), polymeric amide or polyvinyl alcohol.
Further, described macromolecular compound and the weight ratio of Graphite Powder 99 are 1:100-100:1; Described micro-capsule graphene composite material and the weight ratio of pesticide active ingredient are 1:100-100:1.
Further, described micro-capsule graphene composite material controlled release fertilizer granules, is made up of the raw material of following weight percent: female powder 0.1-70%, inorganic nutrients 10-40%, organic 10-50%, hardening resisting agent 1-20%, filler supplies 100%.
Described pesticide active ingredient, comprise sterilant or sterilant, described sterilant is at least one in Rynaxypyr, cyanogen insect amide, ethiprole, Cupric sulfate, disosultap, cartap, clothianidin, Provado, Diacloden, pymetrozine or Ti304; Described sterilant is at least one of tricyclazole, isoprothiolane, tebuconazole, Wocosin 50TK, difenoconazole, thiophanate_methyl, own azoles alcohol, pyraclostrobin, thifluzamide, triadimenol, Azoxystrobin or flutriafol.
Described inorganic nutrients is at least one in single azophoska, composite fertilizer or medium trace element fertilizer.
Described organic matter comprises at least one of filter mud of sugarcane, Chicken dung, osthole, print chinaberry extract, biological nicotine, xanthohumic acid, amino acid or Lalgine.
Described hardening resisting agent is at least one in epoxy resin, polyacrylic resin, resol or polystyrene.
Described filler is at least one in zeolite, carbon black, molecular sieve, kaolin or attapulgite.
The preparation method of described fertilizer granules, comprises following concrete steps:
(1) after pesticide active ingredient and Graphite Powder 99 fully being mixed, micronizer mill is crossed, obtained medicinal powder A;
(2) medicinal powder A, macromolecular compound liquid medium and abrading-ball are placed in ball mill, carry out mechanical mill, obtain mixing suspension; Then by the method for condensing, separate out or be polymerized, obtain the mixture of micro-capsule graphene composite material and pesticide active ingredient, after drying, namely obtain female powder;
(3) female powder, inorganic nutrients, organic matter and filler are added granulation in roller pelletizer, drying; obtain particulate matter; finally the toluene solution of hardening resisting agent is sprayed onto above-mentioned particulate matter, stirs and obtain micro-capsule graphene composite material controlled release fertilizer granules.
The present invention is that my corporate team is through arduous tackling key problem in a few years, develop novel easy degraded macromolecular mould material-micro-capsule graphene composite material, this material solve the fertile Pesticides of medicine and fertilizer compatibleness poor, the fertile poor stability of medicine, agricultural chemicals and the fertilizer lasting period short, the problems such as utilization ratio is low, and the effect simultaneously playing slowly-releasing to agricultural chemicals and fertilizer.The present invention utilizes the interphase interaction of agricultural chemicals and macromolecular compound, and agricultural chemicals is slowly released at reasonable time, can improve biological activity, Co ntrolled release speed, reduce dosage and extend spraying cycle, reduce the infringement to farm crop and environmental pollution, cover the bad stink of medicine; Prevent the volatilization loss of medicine.Fertilizer granules of the present invention is used after rice striking root, applied once, and what can solve whole season uses fertile and disease and pest problem.
Embodiment
Technical scheme of the present invention and beneficial effect is further illustrated below by specific embodiment.The present invention is apart from outside Special Statement, and described degree is weight percent content.
The sustained drug release effect determination test of one micro-capsule graphene composite material
1. test is arranged: prepare female powder sample 1#-60# according to the formula described in following table 1-table 4 respectively, prepare control sample 61#-65# according to the formula described in table 5.
Table 1 test arranges group female powder used and prepares formula table 1 (unit: g)
| Raw material | 1# | 2# | 3# | 4# | 5# | 6# | 7# | 8# | 9# | 10# | 11# | 12# | 13# | 14# | 15# |
| Graphite Powder 99 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 |
| Gelatin | 20 | 50 | 1 | 0.5 | 200 | / | / | / | / | / | / | / | / | / | / |
| Gum arabic | / | / | / | / | / | 100 | 0.1 | 10 | 50 | 2 | / | / | / | / | / |
| Lalgine | / | / | / | / | / | / | / | / | / | / | 100 | 20 | 50 | 0.1 | 1 |
| Clothianidin | 10 | 10 | 10 | 10 | 10 | 10 | 10 | 10 | 10 | 10 | 10 | 10 | 10 | 10 | 10 |
Table 2 test arranges group female powder used and prepares formula table 2 (unit: g)
Table 3 test arranges group female powder used and prepares formula table 3 (unit: g)
| Raw material | 31# | 32# | 33# | 34# | 35# | 36# | 37# | 38# | 39# | 40# | 41# | 42# | 43# | 44# | 45# |
| Graphite Powder 99 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 |
| Polyvinyl alcohol | 10 | 30 | 0.1 | 2 | 300 | 100 | / | / | / | / | / | / | / | / | 1 |
| Starch | / | / | / | / | / | / | 20 | 50 | 0.5 | 5 | 200 | 100 | 0.1 | 2 | 1 |
| Clothianidin | 10 | 10 | 10 | 10 | 10 | 10 | 10 | 10 | 10 | 10 | 10 | 10 | 10 | 10 | 10 |
Table 4 test arranges group female powder used and prepares formula table 4 (unit: g)
Table 5 test arranges group control sample formula table (unit: g) used
| Raw material | 61# | 62# | 63# | 64# | 65# |
| Graphene oxide | 5 | 10 | 50 | / | 5 |
| Chitosan | / | / | / | 10 | 10 |
| Clothianidin | 10 | 10 | 10 | 10 | 10 |
The preparation method of above-mentioned female powder sample is: after fully being mixed with Graphite Powder 99 by clothianidin, crosses comminution by gas stream, obtained medicinal powder A; Medicinal powder A and macromolecular compound liquid medium and abrading-ball are placed in ball mill, carry out mechanical mill, obtain mixing suspension; By the method for above-mentioned mixing suspension by cohesion, obtain the mixture of micro-capsule graphene composite material and pesticide active ingredient, after drying, namely obtain female powder.
The preparation method of above-mentioned control sample is: after fully being mixed with graphene oxide or chitosan by clothianidin, crosses comminution by gas stream and get final product.
This test is also provided with the former medicine of clothianidin 66# in contrast.
2. test method and result
Get above-mentioned 60 female powder samples and 6 control samples of the identical amount of clothianidin effective constituent, after mixing with the pedotheque of equivalent, under being placed in room temperature condition.Respectively at soil sampling after 1 day, 3 days, 7 days, 10 days, 20 days, 30 days, 60 days and 90 days, with indoor feeding aptery become aphid do Contact toxicity determination experiment, measure the mortality ratio after 24h.Result statistics is as shown in table 6 below.
Table 6 each sample is for the Contact toxicity measurement result (mortality ratio: %) of aptery one-tenth aphid
2. interpretation of result
From the result shown in table 6, utilize female powder that micro-capsule graphene composite material of the present invention and pesticide active ingredient are mixed with, release is stable, and the lasting period is long.
Two products prepare embodiment
Prove through more indoor measurement test, the weight ratio of micro-capsule graphene composite material of the present invention and pesticide active ingredient is 1:100-100:1, and pesticide active ingredient all can Stable Release.Described micro-capsule graphene composite material controlled release fertilizer granules, is made up of the raw material of following weight percent: female powder 0.1-70%, inorganic nutrients 10-40%, organic 10-50%, hardening resisting agent 1-20%, when filler supplies 100%, pesticide active ingredient and fertilizer all can Stable Releases.
Pesticide active ingredient of the present invention, can comprise sterilant or sterilant according to actual needs, described sterilant is at least one in Rynaxypyr, cyanogen insect amide, ethiprole, Cupric sulfate, disosultap, cartap, clothianidin, Provado, Diacloden, pymetrozine or Ti304; Described sterilant is at least one of tricyclazole, isoprothiolane, tebuconazole, Wocosin 50TK, difenoconazole, thiophanate_methyl, own azoles alcohol, pyraclostrobin, thifluzamide, triadimenol, Azoxystrobin or flutriafol.Described inorganic nutrients is at least one in single azophoska, composite fertilizer or medium trace element fertilizer.Described organic matter comprises at least one of filter mud of sugarcane, Chicken dung, osthole, print chinaberry extract, biological nicotine, xanthohumic acid, amino acid or Lalgine.Described hardening resisting agent is at least one in epoxy resin, polyacrylic resin, resol or polystyrene.Described filler is at least one in zeolite, carbon black, molecular sieve, kaolin or attapulgite.Said components all can prepare the stable fertilizer granules of release according to preparation method of the present invention.Below only list several concrete product embodiments to be explained.
Product prepares embodiment 1:
(1) get Cupric sulfate 10kg, pymetrozine 1kg, Azoxystrobin 1kg, Graphite Powder 99 20kg, fully after mixing, cross comminution by gas stream, obtained medicinal powder A.
(2) medicinal powder A, chitosan liquid medium, abrading-ball are placed in ball mill, carry out mechanical mill, obtain mixing suspension; By the method for above-mentioned mixing suspension by cohesion, obtain the mixture of micro-capsule graphene composite material and pesticide active ingredient, after drying, namely obtain female powder;
(3) preparation (to produce 1000Kg) of the fertile particle of medicine: get urea 300Kg; ammonium sulfate 100Kg, an ammonium 150Kg, Repone K 200Kg; borax 10Kg; filter mud of sugarcane 100kg, potassium fulvate 2.5kg, above-mentioned female powder 20Kg; kaolin is supplied; add granulation in roller pelletizer, drying, finally the toluene solution of epoxy resin is sprayed onto above-mentioned particle, stir and obtain micro-capsule graphene composite material controlled release fertilizer granules.
Product prepares embodiment 2:
(1) get Rynaxypyr 500g, Diacloden 1kg, difenoconazole 1kg, Graphite Powder 99 20kg, fully after mixing, cross comminution by gas stream, obtained medicinal powder A.
(2) medicinal powder A, starch liquid medium, abrading-ball are placed in ball mill, carry out mechanical mill, obtain mixing suspension; By the method for above-mentioned mixing suspension by cohesion, obtain the mixture of micro-capsule graphene composite material and pesticide active ingredient, after drying, namely obtain female powder;
(3) preparation (to produce 1000Kg) of the fertile particle of medicine: get urea 250Kg, ammonium sulfate 100Kg, two ammonium 100Kg; Repone K 230Kg, borax 10Kg, above-mentioned female powder 20Kg; Chicken dung, 100kg; potassium fulvate 1.5kg, biological nicotine 1kg, Lalgine 1kg; carbon black is supplied; add granulation in roller pelletizer, drying, finally the toluene solution of polystyrene resin is sprayed onto above-mentioned particle, stir and obtain micro-capsule graphene composite material controlled release fertilizer granules.
Product prepares embodiment 3:
(1) get ethiprole 1kg, Ti304 0.75kg, tricyclazole 3Kg, thifluzamide 0.6Kg, Graphite Powder 99 20kg, fully after mixing, cross comminution by gas stream, obtained medicinal powder A.
(2) medicinal powder A, methylcellulose gum liquid medium, abrading-ball are placed in ball mill, carry out mechanical mill, obtain mixing suspension; By the method for above-mentioned mixing suspension by cohesion, obtain the mixture of micro-capsule graphene composite material and pesticide active ingredient, after drying, namely obtain female powder;
(3) preparation (to produce 1000Kg) of the fertile particle of medicine: get urea 300Kg, calcium superphosphate 200Kg, Repone K 200Kg; fused(calcium magnesium)phosphate 200Kg; borax 10Kg, filter mud of sugarcane 100kg, potassium fulvate 2.5kg; osthole 8kg; above-mentioned female powder 20Kg, attapulgite is supplied, and adds granulation in roller pelletizer, drying; finally the toluene solution of epoxy resin is sprayed onto above-mentioned particle, stirs and obtain micro-capsule graphene composite material controlled release fertilizer granules.
Product prepares embodiment 4:
(1) get cyanogen insect amide 1Kg, Provado 5kg, thiophanate_methyl 10Kg, own azoles alcohol 1Kg, Graphite Powder 99 20kg, fully after mixing, cross comminution by gas stream, obtained medicinal powder A.
(2) medicinal powder A, polyvinyl alcohol liquid medium, abrading-ball are placed in ball mill, carry out mechanical mill, obtain mixing suspension; By the method for above-mentioned mixing suspension by cohesion, obtain the mixture of micro-capsule graphene composite material and pesticide active ingredient, after drying, namely obtain female powder;
(3) preparation (to produce 1000Kg) of the fertile particle of medicine: get urea formaldehyde urea 350Kg (commercial); one ammonium 200Kg; potassium sulfate 200Kg, borax 10Kg, filter mud of sugarcane 100kg; potassium fulvate 2.5kg; the above-mentioned female powder 20Kg of biological nicotine 5kg, molecular sieve is supplied, and adds granulation in roller pelletizer, drying; finally the toluene solution of epoxy resin is sprayed onto above-mentioned particle, stirs and obtain micro-capsule graphene composite material controlled release fertilizer granules.
Product prepares embodiment 5:
(1) get cartap 10kg, Diacloden 1kg, Wocosin 50TK 1kg, pymetrozine 1kg, Graphite Powder 99 20kg, fully after mixing, cross comminution by gas stream, obtained medicinal powder A.
(2) medicinal powder A, starch liquid medium, abrading-ball are placed in ball mill, carry out mechanical mill, obtain mixing suspension; By the method for above-mentioned mixing suspension by cohesion, obtain the mixture of micro-capsule graphene composite material and pesticide active ingredient, after drying, namely obtain female powder;
(3) preparation (to produce 1000Kg) of the fertile particle of medicine: humic acids 500Kg; water glass 40Kg; zinc sulfate 20Kg; calcium sulfate 50Kg; zeolite 100Kg; borax 10Kg; above-mentioned female powder 20Kg, Chicken dung, 100kg, potassium fulvate 1.5kg; print chinaberry extract 1kg; Lalgine 1kg, kaolin is supplied, and adds granulation in roller pelletizer, drying; finally the toluene solution of polystyrene resin is sprayed onto above-mentioned particle, stirs and obtain micro-capsule graphene composite material controlled release fertilizer granules.
Three products are in the Application Example in field
The said products is tested at Qiezhou little Dong, every mu of rice terrace uses 30Kg, after rice transplanting is turned green, apply when base fertilizer is disposable, later stage does not go and buy Chinese medicine, and compares (every mu, base fertilizer use 20Kg 45% composite fertilizer, rear additional 5Kg urea with peasant household is traditional with fertile medication, conventional dispenser 3 times), test-results is as shown in table 7 below.
The each product effect comparison (%) of table 7
| Sample | Borer preventive effect | Tortrix moth preventive effect | Banded sclerotial blight preventive effect | Planthopper preventive effect | Stimulation ratio * |
| Embodiment 1 | 86.7 | 92.7 | 78.2 | 98.6 | 5.2 |
| Embodiment 2 | 85.3 | 95.3 | 77.5 | 97.5 | 4.9 |
| Embodiment 3 | 88.3 | 88.3 | 79.3 | 92.7 | 8.6 |
| Embodiment 4 | 85.1 | 89.1 | 66.8 | 90.1 | 7.8 |
| Embodiment 5 | 82.8 | 87.8 | 75.9 | 92.3 | 5.3 |
| Tradition | 85.4 | 89.4 | 70.2 | 90.8 | — |
* relative to the fertile medication of tradition
The borer of each embodiment sample, tortrix moth, banded sclerotial blight, planthopper preventive effect can reach control requirement as can be seen from Table 7, and there is the preventive effect of individual samples to be better than conventional application method, each sample process all has the effect of volume increase, illustrates that the lasting period of fertilizer is also extended.
In sum, micro-capsule graphene composite material controlled release medicine fertilizer can realize the Co ntrolled release simultaneously to fertilizer and agricultural chemicals, and need not refertilize in a dispenser whole season spray medicine, and anti-usefulness arrives control requirement, and can also increase production, and has boundless application prospect.
Claims (10)
1. a micro-capsule graphene composite material controlled release fertilizer granules, is characterized in that, is made up of female powder, inorganic nutrients, organic matter, hardening resisting agent and filler;
Described female powder is made up of micro-capsule graphene composite material and pesticide active ingredient;
Described micro-capsule graphene composite material is composited by macromolecular compound and Graphite Powder 99, and described macromolecular compound is at least one in gelatin, gum arabic, starch, chitosan, Lalgine, methylcellulose gum, carboxymethyl cellulose salt, poly(lactic acid), polymeric amide or polyvinyl alcohol.
2. micro-capsule graphene composite material controlled release fertilizer granules according to claim 1, it is characterized in that, described macromolecular compound and the weight ratio of Graphite Powder 99 are 1:100-100:1.
3. micro-capsule graphene composite material controlled release fertilizer granules according to claim 1, is characterized in that, described micro-capsule graphene composite material and the weight ratio of pesticide active ingredient are 1:100-100:1.
4. micro-capsule graphene composite material controlled release fertilizer granules according to claim 1, it is characterized in that, described micro-capsule graphene composite material controlled release fertilizer granules, be made up of the raw material of following weight percent: female powder 0.1-70%, inorganic nutrients 10-40%, organic 10-50%, hardening resisting agent 1-20%, filler supplies 100%.
5. the micro-capsule graphene composite material controlled release fertilizer granules according to any one of claim 1-4, it is characterized in that, described pesticide active ingredient, comprise sterilant or sterilant, described sterilant is at least one in Rynaxypyr, cyanogen insect amide, ethiprole, Cupric sulfate, disosultap, cartap, clothianidin, Provado, Diacloden, pymetrozine or Ti304; Described sterilant is at least one of tricyclazole, isoprothiolane, tebuconazole, Wocosin 50TK, difenoconazole, thiophanate_methyl, own azoles alcohol, pyraclostrobin, thifluzamide, triadimenol, Azoxystrobin or flutriafol.
6. the micro-capsule graphene composite material controlled release fertilizer granules according to any one of claim 1-4, is characterized in that, described inorganic nutrients is at least one in single azophoska, composite fertilizer or medium trace element fertilizer.
7. the micro-capsule graphene composite material controlled release fertilizer granules according to any one of claim 1-4, it is characterized in that, described organic matter comprises at least one of filter mud of sugarcane, Chicken dung, osthole, print chinaberry extract, biological nicotine, xanthohumic acid, amino acid or Lalgine.
8. the micro-capsule graphene composite material controlled release fertilizer granules according to any one of claim 1-4, it is characterized in that, described hardening resisting agent is at least one in epoxy resin, polyacrylic resin, resol or polystyrene.
9. the micro-capsule graphene composite material controlled release fertilizer granules according to any one of claim 1-4, it is characterized in that, described filler is at least one in zeolite, carbon black, molecular sieve, kaolin or attapulgite.
10. the preparation method of the micro-capsule graphene composite material controlled release fertilizer granules according to any one of claim 1-4, is characterized in that, comprise following concrete steps:
(1) after pesticide active ingredient and Graphite Powder 99 fully being mixed, micronizer mill is crossed, obtained medicinal powder A;
(2) medicinal powder A, macromolecular compound liquid medium and abrading-ball are placed in ball mill, carry out mechanical mill, obtain mixing suspension; Then by the method for condensing, separate out or be polymerized, obtain the mixture of micro-capsule graphene composite material and pesticide active ingredient, after drying, namely obtain female powder;
(3) female powder, inorganic nutrients, organic matter and filler are added granulation in roller pelletizer, drying; obtain particulate matter; finally the toluene solution of hardening resisting agent is sprayed onto above-mentioned particulate matter, stirs and obtain micro-capsule graphene composite material controlled release fertilizer granules.
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