CN106278764B - Method for preparing compound fertilizer containing microcapsule type fertilizer synergist and prepared compound fertilizer - Google Patents
Method for preparing compound fertilizer containing microcapsule type fertilizer synergist and prepared compound fertilizer Download PDFInfo
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- CN106278764B CN106278764B CN201610644389.2A CN201610644389A CN106278764B CN 106278764 B CN106278764 B CN 106278764B CN 201610644389 A CN201610644389 A CN 201610644389A CN 106278764 B CN106278764 B CN 106278764B
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
- C05G3/90—Mixtures of one or more fertilisers with additives not having a specially fertilising activity for affecting the nitrification of ammonium compounds or urea in the soil
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01G—HORTICULTURE; CULTIVATION OF VEGETABLES, FLOWERS, RICE, FRUIT, VINES, HOPS OR SEAWEED; FORESTRY; WATERING
- A01G17/00—Cultivation of hops, vines, fruit trees, or like trees
- A01G17/005—Cultivation methods
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01G—HORTICULTURE; CULTIVATION OF VEGETABLES, FLOWERS, RICE, FRUIT, VINES, HOPS OR SEAWEED; FORESTRY; WATERING
- A01G22/00—Cultivation of specific crops or plants not otherwise provided for
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01G—HORTICULTURE; CULTIVATION OF VEGETABLES, FLOWERS, RICE, FRUIT, VINES, HOPS OR SEAWEED; FORESTRY; WATERING
- A01G22/00—Cultivation of specific crops or plants not otherwise provided for
- A01G22/20—Cereals
- A01G22/22—Rice
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B7/00—Fertilisers based essentially on alkali or ammonium orthophosphates
Abstract
The invention provides a method for preparing a compound fertilizer containing a microcapsule type fertilizer synergist, which is characterized in that the microcapsule type fertilizer synergist is added in the process of preparing the compound fertilizer by a melting method, wherein the effective component in the microcapsule type fertilizer synergist is 2-chloro-6-trichloromethyl pyridine, the temperature of slurry during adding is 80-250 ℃, and the dispersion time after adding the microcapsule type fertilizer synergist into the slurry is 0.1-120 min. The invention also provides a compound fertilizer prepared by the method and an application and application method thereof.
Description
Technical Field
The invention belongs to the field of novel fertilizers, and particularly relates to a method for preparing a compound fertilizer containing a microcapsule type fertilizer synergist, namely a method for preparing a stable fertilizer by adding the microcapsule type fertilizer synergist in the process of producing the compound fertilizer by a melting method. In addition, the invention also relates to a compound fertilizer containing the microcapsule type fertilizer synergist prepared by the method and an application and application method thereof.
Background
Nitrogen is an essential nutrient for plants and plays an extremely important role. As an important source of nitrogen fertilizers, both amide nitrogen and ammonium nitrogen undergo a process in soil in which ammonium nitrogen is oxidized into nitrite nitrogen, and further oxidized into nitrate nitrogen by nitrifying bacteria. According to the presently disclosed study, the amide nitrogen entering the soil is converted into ammonium nitrogen in 3-7 days, and 80% of the nitrogen is converted into nitrate nitrogen in 15-20 days. Nitrate nitrogen is not easy to be adsorbed in soil and is easy to be leached and lost, so that the utilization rate of the whole nitrogen fertilizer is low, and greenhouse gas is discharged.
The method is an effective means for improving the utilization rate of nitrogen fertilizers in the fertilizer industry by adding nitrification inhibitors to inhibit the conversion of ammonium nitrogen into nitrate nitrogen, 2-chloro-6-trichloromethylpyridine is an active ingredient with the highest inhibition rate on nitrobacteria which is commercialized at present, and a plurality of documents report related formulations and application methods in fertilizers.
CN102976857 discloses a method of adding 2-chloro-6-trichloromethylpyridine to an organic solvent and an anti-caking agent, followed by addition of urea. CN103524272 discloses a method for adding 2-chloro-6-trichloromethyl pyridine into compound fertilizer by a high tower granulation method, and the two methods are that active ingredients are directly added into urea or compound fertilizer, and the active ingredients are easy to volatilize and decompose.
CN102249817 discloses 2-chloro-6-trichloromethyl pyridine in the form of emulsifiable concentrate, but the application range of the method is small, and the solvent in the emulsifiable concentrate has adverse effect on the environment.
US20080176745 and US20090227458 of the dow bengal agriculture disclose methods for preparing 2-chloro-6-trichloromethyl pyridine into microcapsule suspending agents (namely, microcapsule type fertilizer synergists), and a commercial product Entrench (Chinese name: companions) is prepared, is directly used for field application or used in tank mixing, and has a lasting period of 60 days in soil. CN104262065 discloses a method of adding a commercial microcapsule suspension product into a compound fertilizer by an extrusion granulation method, wherein the preparation method comprises mixing the microcapsule suspension product with a part of fertilizer raw materials by a spraying process, then mixing with the rest of the fertilizer raw materials, and obtaining the compound fertilizer by the extrusion granulation method. The method disperses the microcapsule synergist in the compound fertilizer, but adds a spraying process in the production process, thereby increasing the equipment and operation cost, and the extrusion method for producing the compound fertilizer also has the serious problems of relatively low production efficiency, uneven dispersion of raw materials and irregular fertilizer particles.
In the current and foreseeable future, solid fertilizers are still the dominant in fertilizer application. The development of a high-quality, environment-friendly and efficient solid compound fertilizer technology is an important guarantee for promoting agricultural development and realizing the reduction and the increase of fertilizers, and is also an aim which is always realized by the technical personnel in the field.
Disclosure of Invention
In order to solve the problems existing in the prior art:
an object of the present invention is to provide a method for preparing a novel compound fertilizer containing a microcapsule-type fertilizer synergist by adding the microcapsule-type fertilizer synergist to the fertilizer using a compound fertilizer production process of a melting method.
Another object of the present invention is to provide a novel compound fertilizer containing a microcapsule type fertilizer synergist.
It is a further object of the present invention to provide the use of a compound fertilizer containing a microcapsule-type fertilizer synergist.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the invention provides a method for preparing a compound fertilizer containing a microcapsule type fertilizer synergist, which is characterized in that the microcapsule type fertilizer synergist is added in the process of preparing the compound fertilizer by a melting method, the effective component in the microcapsule type fertilizer synergist is 2-chloro-6-trichloromethyl pyridine, the temperature of slurry during adding is 80-250 ℃, and the dispersion time of the microcapsule type fertilizer synergist after being added into the slurry is 0.1-120 min.
Preferably, the slurry temperature is 105 ℃ to 230 ℃, and the dispersion time is 0.2 to 3 min.
Preferably, cooling is performed after the dispersing.
Preferably, the content range of the microcapsule type fertilizer synergist is 0.0001-5% of 2-chloro-6-trichloromethyl pyridine in terms of 100% by mass of the compound fertilizer, the nitrogen content of the compound fertilizer is 1-46%, the phosphorus pentoxide content of the compound fertilizer is 0-30%, and the potassium oxide content of the compound fertilizer is 0-30%.
Preferably, the content of the microcapsule type fertilizer synergist is 0.001-5% in terms of 100% of 2-chloro-6-trichloromethylpyridine, relative to the mass percent of the compound fertilizer, the nitrogen content of the compound fertilizer is 15-40%, the phosphorus pentoxide content of the compound fertilizer is 5-25%, and the potassium oxide content of the compound fertilizer is 5-25%.
Preferably, the compound fertilizer also contains medium trace elements, wherein 0-15% of magnesium, 0-15% of calcium, 0-30% of sulfur, 0-10% of zinc, 0-5% of boron, 0-5% of manganese, 0-5% of iron, 0-5% of copper and 0-0.5% of molybdenum by mass percentage.
Preferably, the compound fertilizer comprises, by mass, 0-10% of magnesium, 0-10% of calcium, 0-20% of sulfur, 0-8% of zinc, 0-3% of boron, 0-2% of manganese, 0-2% of iron, 0-2% of copper and 0-0.3% of molybdenum.
Further, the invention provides a compound fertilizer containing the microcapsule type fertilizer synergist prepared by the method.
Further, the invention provides a blended fertilizer, a leaf fertilizer, a liquid fertilizer or a water-soluble fertilizer, which contains the compound fertilizer containing the microcapsule type fertilizer synergist.
Further, the invention provides a method for applying the compound fertilizer containing the microcapsule type fertilizer synergist, which is characterized in that the compound fertilizer is directly applied to crops or applied to the crops after being used as a raw material to produce a bulk fertilizer, a foliar fertilizer, a liquid fertilizer and a water soluble fertilizer, wherein the application mode is bottom application, top application, hole application or foliar spraying.
Further, the invention provides application of the compound fertilizer containing the microcapsule type fertilizer synergist, which is characterized in that the compound fertilizer is applied to crops in agriculture, forestry and grass industry.
Preferably, the agricultural crop is selected from cucumber, tomato, celery, potato, sunflower, strawberry, corn, rice, wheat and sugar cane, the forestry crop is selected from fruit trees, pear trees, orange trees, pine trees, poplar trees, flowers and the grassy crop is selected from lawn.
Detailed description of the invention:
the microcapsule type fertilizer synergist is a microcapsule suspending agent of 2-chloro-6-trichloromethylpyridine, and the preparation method of the microcapsule type fertilizer synergist is known in the field. For example, US20080176745 and US20090227458 disclose that the wall materials of the microcapsule are isocyanate and polyamine, and are prepared by interfacial polymerization, and in the preparation reaction, a thickening agent, an emulsifier, a dispersing agent and a biocide are contained. CN103044137 discloses that 1-60 parts of 2-chloro-6-trichloromethyl pyridine, 1-15 parts of capsule wall material, 0.05-0.3 part of viscosity regulator, 2-10 parts of dispersant and 0.1-100 parts of water are used for preparing microcapsule suspending agent by adopting an emulsion polymerization method. The content of 2-chloro-6-trichloromethylpyridine is wide, typically in the range of 1-70% relative to the mass of the microcapsule suspension, for example 17.67% for 2-chloro-6-trichloromethylpyridine in Entrench (companion), a commercial product of Yinong Dow.
In the invention, after the capsule suspending agent added in the compound fertilizer is converted into 100% of 2-chloro-6-trichloromethyl pyridine, the adding amount of the capsule suspending agent is 0.0001-5% by mass percent, and further 0.001-5% by mass percent relative to the mass of the compound fertilizer.
According to the mass percent, the nitrogen content in the compound fertilizer is 1-46%, further 15-40%, wherein the nitrogen element can be one, two, three or a mixture of four of amide nitrogen, ammonium nitrogen, nitrate nitrogen and organic nitrogen in any proportion. The source of nitrogen element is nitrogen-containing substances for agricultural use, such as urea, aqueous ammonia, synthetic ammonia, ammonium hydrogen carbonate, ammonium sulfate, ammonium hydrogen sulfate, ammonium dihydrogen phosphate, diammonium hydrogen phosphate, ammonium nitrate, potassium nitrate, ammonium polyphosphate, organic nitrogen and the like.
In the present invention, the phosphorus pentoxide content in the compound fertilizer is 0 to 30% by mass, further 5 to 25% by mass, and the phosphorus source is a phosphorus-containing substance for agricultural use, such as monoammonium phosphate, diammonium phosphate, monopotassium phosphate, phosphoric acid, polyphosphoric acid, and polyphosphate, and the like.
In the present invention, the content of potassium oxide in the compound fertilizer is 0 to 30% by mass, further 5 to 25% by mass, and the source of potassium is a potassium-containing substance used for agricultural purposes, such as potassium sulfate, potassium nitrate, potassium dihydrogen phosphate, potassium chloride, potassium hydroxide, and the like.
The product of the invention can also be added with medium trace elements, wherein, according to the mass percentage, the magnesium is 0-15%, the calcium is 0-15%, the sulfur is 0-30%, the zinc is 0-10%, the boron is 0-5%, the manganese is 0-5%, the iron is 0-5%, the copper is 0-5%, the molybdenum is 0-1%, further, the magnesium is 0-10%, the calcium is 0-10%, the sulfur is 0-20%, the zinc is 0-8%, the boron is 0-3%, the manganese is 0-2%, the iron is 0-2%, the copper is 0-2%, and the molybdenum is 0-0.3%. The boron comprises common disodium tetraborate decahydrate, sodium octaborate tetrahydrate, boric acid and the like, and the rest metal elements comprise chelated elements and ionic elements in various valence states.
In the invention, when the method is adopted to produce the stable fertilizer, the dye can be added or not added.
In the invention, the melting method is that the fertilizer is heated to be in a molten state, the flowable melt is sprayed into a refrigerant, and the material is solidified into granules when being cooled, or the flowable melt is sprayed onto returned particles in a mechanical granulator, so that the particles are coated or bonded on the surfaces of the particles to form the granules.
In the invention, the adding process of the synergist in the compound fertilizer is as follows, adding the microcapsule suspending agent of 2-chloro-6-trichloromethyl pyridine into the fused compound fertilizer slurry, wherein the temperature range of the slurry is 80-250 ℃, and further, 105-. Suspending and dispersing the added microcapsule into the slurry by a mechanical method for 0.1-120min, further 0.2-3min, and cooling to obtain the compound fertilizer product. In the actual production of fertilizers by the melt process, granulation may also be performed before cooling.
The application modes of the compound fertilizer product prepared by the invention comprise application modes such as bottom application, topdressing, hole application, foliar spraying and the like. The compound fertilizer product prepared by the invention can be directly applied, and can also be used as a fertilizer raw material for producing blended fertilizers, compound fertilizers, foliar fertilizers, liquid fertilizers and water-soluble fertilizers and then applied.
The compound fertilizer product prepared by the invention can be applied to crops, wherein the crops comprise agricultural, forestry and grassy crops with economic and social values, the agricultural economic crops comprise cucumbers, tomatoes, celery, potatoes, sunflowers, strawberries and the like, the field crops comprise corns, rice, wheat and the like, the forestry comprises various trees, flowers and the like, and the forestry comprises lawns and the like.
In the present invention, the sample prepared by the disclosed method can be quantitatively analyzed by using analytical instruments such as gas chromatograph and liquid chromatograph, and the retention ratio in the present invention is defined as follows:
the retention rate is × 100% of the actual content of 2-chloro-6-trichloromethylpyridine tested/theoretical calculation value.
The invention has the technical effects that:
the preparation process for producing the stable fertilizer by the melting method disclosed by the invention is to uniformly, stably and conveniently disperse the microcapsule type fertilizer synergist containing the 2-chloro-6-trichloromethylpyridine in the solid fertilizer, so that the preparation process has the remarkable advantages of high production efficiency, short process, no adverse effect on the environment and low production cost, and overcomes the problems in the prior art.
Because the 2-chloro-6-trichloromethyl pyridine in the obtained stable fertilizer product is uniformly added into the fertilizer in a microcapsule form, the active ingredients are ensured not to be easily volatilized in the production, storage and transportation processes, and the active ingredients are isolated from the fertilizer through the microcapsule wall, so that the decomposition and deterioration of the active ingredients are avoided.
When the effective components are applied to the soil along with the fertilizer, the effective components exist in the microcapsules, so that the effective period of the effective components in the soil is guaranteed, the effective components are uniformly mixed with the fertilizer in a microcapsule form, the soil is guaranteed to have better convenience and accuracy, and the fertilizer has the remarkable advantages of long effective time and no fertilizer release in the later growth stage of crops.
The above and other objects, advantages and features of the present invention will become more apparent to those skilled in the art from the following detailed description of specific embodiments thereof, but the present invention is not limited to these specific embodiments.
Detailed Description
The starting materials and equipment used in the examples are well known to those skilled in the art and are either commercially available or readily available or manufactured.
Example 1
100g of industrial grade urea is weighed and heated and melted at the temperature of 150 ℃. 50g (11-44-0) of powdery ammonium dihydrogen phosphate and 50g (0-0-60) of potassium chloride are weighed, dried for 30min at the temperature of 70 ℃, added into urea melt, rapidly stirred to form uniform slurry, the temperature of the slurry is 120 ℃, 1.05g of microcapsule suspending agent (for example, energy tracing) with the content of 2-chloro-6-trichloromethyl pyridine of 17.67 percent is added, rapidly stirred for 2min and cooled to obtain the compound fertilizer product containing the 2-chloro-6-trichloromethyl pyridine microcapsules. The nitrogen content of the compound fertilizer is 25.9 percent, the phosphorus pentoxide content is 10.9 percent, the potassium oxide content is 14.9 percent, and the theoretical content of the 2-chloro-6-trichloromethylpyridine is 0.092 percent.
The content of 2-chloro-6-trichloromethylpyridine is analyzed by a gas chromatograph, the retention rate is 95.5% relative to theoretical calculation, the sample is stored for 14 days at the temperature of 54 +/-2 ℃, and the retention rate of effective components relative to the theoretical content is 71.4%.
Example 2
Weighing 100g of industrial grade urea, heating and melting at 150 ℃, drying a mixture of 50g (12-61-0) of powdery ammonium dihydrogen phosphate, 50g (0-0-54) of potassium sulfate, 1g of zinc sulfate heptahydrate and 0.8g of disodium tetraborate decahydrate at 70 ℃ for 30min, adding the mixture into urea molten liquid, quickly stirring the mixture to form uniform slurry, wherein the slurry temperature is 110 ℃, adding 0.5g of microcapsule suspending agent with the 2-chloro-6-trichloromethyl pyridine content of 17.67 percent, quickly stirring the slurry for 3min, cooling to obtain a compound fertilizer product containing the 2-chloro-6-trichloromethyl pyridine microcapsules, wherein the nitrogen content in the compound fertilizer is 26 percent, the phosphorus pentoxide content is 15.1 percent, the potassium oxide content is 13.3 percent, and the theoretical content of the 2-chloro-6-trichloromethyl pyridine is 0.044 percent, 0.11 percent of zinc and 0.04 percent of boron.
The content of 2-chloro-6-trichloromethylpyridine is analyzed by using a gas chromatograph, the retention rate is 84.1% relative to theoretical calculation, the sample is stored for 14 days at the temperature of 54 +/-2 ℃, and the retention rate of the effective components is 64.9% relative to theoretical calculation.
Example 3
Weighing 100g of industrial-grade urea, heating and melting at 150 ℃, drying a mixture of 40g (12-61-0) of powdery ammonium dihydrogen phosphate, 60g (0-0-60) of potassium chloride, 5g of magnesium sulfate heptahydrate, 2.5g of EDTA-Ca, 1.5g of EDTA-Zn, 0.8g of EDTA-Mn, 0.5g of EDTA-Fe, 0.5g of EDTA-Cu, 0.1g of ammonium molybdate and 0.5g of sodium octaborate tetrahydrate at 70 ℃ for 30min, adding the mixture into a urea molten liquid, quickly stirring the mixture to form uniform slurry, adding 1.5g of a microcapsule suspending agent containing 17.67% of 2-chloro-6-trichloromethylpyridine at the temperature of 125 ℃, quickly stirring the slurry for 2min, and cooling to obtain a product containing the 2-chloro-6-trichloromethylpyridine microcapsule, wherein the nitrogen content in the compound fertilizer is 24.3%, 11.5 percent of phosphorus pentoxide, 17.0 percent of potassium oxide, 0.125 percent of theoretical content of 2-chloro-6-trichloromethyl pyridine, 0.23 percent of magnesium, 0.12 percent of calcium, 0.01 percent of zinc, 0.05 percent of manganese, 0.03 percent of iron, 0.04 percent of copper, 0.02 percent of molybdenum and 0.05 percent of boron.
The content of 2-chloro-6-trichloromethylpyridine was analyzed by gas chromatography, and the retention rate was 86.8% relative to the theoretical content.
Example 4
Weighing 100g of industrial-grade urea, heating and melting at 150 ℃, drying a mixture of 50g (12-61-0) of powdery ammonium dihydrogen phosphate, 50g (0-0-60) of potassium chloride, 5g of magnesium sulfate heptahydrate, 2.5g of EDTA-Ca, 1.5g of EDTA-Zn, 0.8g of EDTA-Mn, 0.5g of EDTA-Fe, 0.5g of EDTA-Cu, 0.1g of ammonium molybdate and 0.5g of sodium octaborate tetrahydrate at 70 ℃ for 30min, adding the mixture into a urea molten liquid, quickly stirring the mixture to form uniform slurry, adding 1.5g of a microcapsule suspending agent containing 17.67% of 2-chloro-6-trichloromethylpyridine at the slurry temperature of 125 ℃, quickly stirring the slurry for 2min, and cooling to obtain a product containing the 2-chloro-6-trichloromethylpyridine microcapsule, wherein the nitrogen content in the compound fertilizer is 24.9%, 14.4 percent of phosphorus pentoxide, 14.2 percent of potassium oxide, 0.125 percent of theoretical content of 2-chloro-6-trichloromethyl pyridine, 0.23 percent of magnesium, 0.12 percent of calcium, 0.01 percent of zinc, 0.05 percent of manganese, 0.03 percent of iron, 0.04 percent of copper, 0.02 percent of molybdenum and 0.05 percent of boron.
The content of 2-chloro-6-trichloromethylpyridine was analyzed by a gas chromatograph, and the retention rate was 86.8% relative to theoretical calculation.
Example 5
In a high tower granulation device, the continuous production of N: P is carried out at the speed of 25 tons/h2O5∶K2The production method of the compound fertilizer with the O being 26: 11 comprises the steps of producing per ton of the compound fertilizer with 501.1kg of industrial urea, 250kg (11-44-0) of ammonium dihydrogen phosphate and 183.3kg (0-0-60) of potassium chloride products and 59.6kg of fillers, adding a microcapsule suspending agent containing 17.67 percent of 2-chloro-6-trichloromethyl pyridine into each ton of the compound fertilizer, wherein the adding amount is 6kg, melting the urea at 140 ℃, introducing the urea into a mixing tank, preheating the ammonium dihydrogen phosphate, the potassium chloride and the fillers at 60 ℃, adding the mixture into a urea molten liquid for mixing, introducing the mixed slurry into another mixing tank, adding the 2-chloro-6-trichloromethyl pyridine microcapsule suspending agent into the mixing tank at the speed of 150kg/h, fully mixing for 3min, spraying the slurry at the tower top of a high tower through a spray nozzle, naturally falling on the tower bottom, forming round grains with the diameter of 1-4 mm. The content of the 2-chloro-6-trichloromethyl pyridine in the fertilizer product is analyzed by using a gas chromatograph, the retention rate is 84.0% by theoretical calculation, the sample is subjected to thermal storage for 14 days at the temperature of 54 +/-2 ℃, and the retention rate of the effective component is 65.8% by theoretical calculation.
Example 6
150g (11-44-0) of powdery ammonium dihydrogen phosphate and 50g (0-0-60) of powdery potassium chloride are heated to 230 ℃ to gradually form a slurry, 0.1g of microcapsule suspending agent with the content of 2-chloro-6-trichloromethyl pyridine of 17.67 percent is added, the mixture is rapidly stirred for 0.2min, and the mixture is rapidly cooled to obtain the compound fertilizer product containing the 2-chloro-6-trichloromethyl pyridine microcapsule. In the compound fertilizer, the nitrogen content is 8.2 percent, the phosphorus pentoxide content is 33.0 percent, the potassium oxide content is 15.0 percent, and the theoretical content of 2-chloro-6-trichloromethyl pyridine is 0.009 percent.
The content of 2-chloro-6-trichloromethylpyridine is analyzed by using a gas chromatograph, the retention rate is 90.1% relative to theoretical calculation, the sample is stored for 14 days at the temperature of 54 +/-2 ℃, and the retention rate of the effective components is 57.2% relative to theoretical calculation.
Example 7
Weighing 200g of industrial urea, heating at 105 ℃, gradually melting, adding 1.5g of EDTA-Zn, adding 40.0g of microcapsule suspending agent containing 17.67% of 2-chloro-6-trichloromethylpyridine, keeping the temperature of slurry at 105 ℃, stirring for 110min, and cooling to obtain 220.5g of zinc-added urea containing 2-chloro-6-trichloromethylpyridine microcapsule suspending agent, wherein the nitrogen content is 42.3%, the zinc content is 0.01%, and the theoretical content of 2-chloro-6-trichloromethylpyridine is 3.2%.
The content of 2-chloro-6-trichloromethylpyridine is analyzed by a liquid chromatograph, and the retention rate is 66.7% relative to theoretical calculation.
Example 8
In a high tower granulation device, the N: P is continuously produced at the speed of 20 tons/h2O5∶K2O＝19∶4∶25The compound fertilizer has the feeding amount of 388.0kg of industrial urea, 91kg (11-44-0) of ammonium dihydrogen phosphate, 471.7kg (0-0-53) of potassium sulfate, 20.2kg of filler, 0.1kg of yellow dye, 5kg of energy accompaniment, 10kg of magnesium sulfate heptahydrate, 9kg of EDTA-Zn and 5kg of sodium octaborate tetrahydrate in each ton of compound fertilizer production, the raw materials except the urea are fully mixed, then preheating at 70 ℃, melting urea at 150 ℃, adding the preheated solid mixture into urea melt for mixing, introducing the mixed slurry into another mixing tank, adding the 2-chloro-6-trichloromethyl pyridine microcapsule suspending agent into a mixing tank at the speed of 100kg/h, fully mixing for 2min, the slurry is sprayed out from the top of the high tower through a spray head and naturally falls to the bottom of the tower to form round particles with the diameter of 1-4 mm. The content of 2-chloro-6-trichloromethylpyridine is analyzed by using a gas chromatograph, the retention rate is 89.8% relative to theoretical calculation, the sample is stored for 14 days at the temperature of 54 +/-2 ℃, and the retention rate of effective components is 69.3% relative to theoretical calculation.
Example 9
The compound fertilizer product of 26-11-11 prepared in example 5 was used as a raw material to prepare a blended fertilizer product of 24-20-6. 545.5kg of the product of example 5, 229.5kg of granular monoammonium phosphate (12-61-0), 152.2kg of large granular urea and 72.8kg of filler were weighed out and mixed in a mixer to obtain a 24-20-6 bulk fertilizer product.
Example 10
In 2015, a corn field test is carried out in the double cities of Heilongjiang, the corn variety is good jade 66, 40kg of the sample in example 5 is applied to each mu, and the control is a blending fertilizer of 26-11-11 without energy accompanying. The quality and yield traits of maize at the staminate stage and after maturation were investigated (see tables 1, 2, 3).
TABLE 1 questionnaire of stamen drawing and silking period
TABLE 2 survey table of maize quality traits
| Treatment of | Ear length (cm) | Line number (cm) | Number of lines and grains |
| Example 5 | 20.98 | 18 | 34.4 |
| Control | 20.90 | 18 | 32.8 |
TABLE 3 corn yield trait survey table
As shown in tables 1, 2 and 3, the treatment yield of example 5 was higher than that of the control treatment, and the yield of example 5 was higher than that of the control by 9.93%. The treatment of example 5 was better than the control treatment in both average ear weight and seed yield.
Example 11
In 2015, different sites were selected, and field experiments were performed in different regions using the product obtained in example 5 to test the effect on yield (see table 4).
TABLE 4 yield of product of example 5 on crop
In the series of trials described above, the average yield increase of the product obtained in example 5 was 19.9% in corn and 11.8% in sunflower, as shown in table 4.
In addition, in various crops, the application (directly or indirectly) of the products obtained in example 5 and other examples is superior to the quality and yield traits (such as average ear weight, seed yield, average yield increase rate and the like) of the crops to the control and the prior art.
As shown in the preparation examples and the effect examples, the process for producing the compound fertilizer containing the microcapsule type fertilizer synergist by the melting method has the remarkable advantages of short production process, high efficiency, no adverse effect on the environment and low production cost, the obtained compound fertilizer is uniform and stable, and the content ratio of each component is optimized by the production process.
The effective components of the compound fertilizer obtained in the embodiment are not easy to volatilize in the production, storage and transportation processes, and when the effective components are applied to soil along with the fertilizer, the compound fertilizer has good convenience and accuracy, and has the remarkable advantages of long lasting time and no fertilizer loss in the later growth period of crops.
Thus, it should be appreciated by those skilled in the art that while a number of exemplary embodiments of the invention have been illustrated and described in detail herein, many other variations or modifications consistent with the principles of the invention may be directly determined or derived from the disclosure of the present invention without departing from the spirit and scope of the invention. Accordingly, the scope of the invention should be understood and interpreted to cover all such other variations or modifications.
Claims (9)
1. A method for preparing a compound fertilizer containing a microcapsule type fertilizer synergist is characterized in that the microcapsule type fertilizer synergist is added in the process of preparing the compound fertilizer by a melting method, the effective component in the microcapsule type fertilizer synergist is 2-chloro-6-trichloromethyl pyridine, the temperature of slurry during adding is 80-250 ℃, and the dispersion time of the microcapsule type fertilizer synergist after being added into the slurry is 0.1-120 min;
relative to the mass percentage of the compound fertilizer, the content range of the microcapsule type fertilizer synergist is 0.001-5% after the microcapsule type fertilizer synergist is converted into 100% of 2-chloro-6-trichloromethylpyridine, the nitrogen content in the compound fertilizer is 15-40%, the phosphorus pentoxide content is 5-25%, and the potassium oxide content is 5-25%;
the compound fertilizer also contains medium trace elements, wherein the mass percentage of magnesium is 0-15%, calcium is 0-15%, sulfur is 0-30%, zinc is 0-10%, boron is 0-5%, manganese is 0-5%, iron is 0-5%, copper is 0-5%, and molybdenum is 0-0.5%.
2. The method as claimed in claim 1, wherein the slurry temperature is 105-230 ℃ and the dispersion time is 0.2-3 min.
3. The method according to claim 1 or 2, characterized in that after the dispersing, cooling is performed.
4. The method according to claim 1, wherein 0-10% by mass of magnesium, 0-10% by mass of calcium, 0-20% by mass of sulfur, 0-8% by mass of zinc, 0-3% by mass of boron, 0-2% by mass of manganese, 0-2% by mass of iron, 0-2% by mass of copper, and 0-0.3% by mass of molybdenum are used as the raw material of the compound fertilizer.
5. Compound fertilizer containing microcapsule-type fertilizer synergists, prepared by the method according to any one of claims 1 to 4.
6. A blended fertilizer, a foliar fertilizer, a liquid fertilizer or a water-soluble fertilizer containing the compound fertilizer containing the microcapsule-type fertilizer synergist according to claim 5.
7. The method for applying a compound fertilizer containing a microcapsule-type fertilizer synergist according to claim 5, wherein the compound fertilizer is directly applied to crops, or applied to crops after being used as a raw material for producing a bulk fertilizer, a foliar fertilizer, a liquid fertilizer and a water-soluble fertilizer, in a manner of bottom application, top application, hole application or foliar spray application.
8. Use of a compound fertilizer containing microcapsule type fertilizer synergist according to claim 5, characterized in that said compound fertilizer is applied to crops in agriculture, forestry and grassy industry.
9. The use according to claim 8, wherein the agricultural crops are selected from the group consisting of cucumber, tomato, celery, potato, sunflower, strawberry, corn, rice, wheat and sugar cane, the forestry crops are selected from the group consisting of fruit trees, pine trees, poplar trees, flowers and grassy crops are selected from the group consisting of turf.
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| CN107285968A (en) * | 2017-07-25 | 2017-10-24 | 张忠庆 | Delay microcapsules suspension formulation of control-release function and its preparation method and application with nitrogenous fertilizer |
| CN112209765B (en) * | 2020-08-17 | 2022-06-07 | 中化化肥有限公司 | Synergist, synergistic potassium fertilizer and preparation method thereof |
| CN112919981A (en) * | 2021-04-13 | 2021-06-08 | 福建恒生态建筑工程有限公司 | Process for composting branches and excrement |
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| CN102807415A (en) * | 2011-05-31 | 2012-12-05 | 上海化工研究院 | Manufacturing method of environment-friendly type controlled-release compound mixed fertilizer |
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