WO2023142473A1 - 一种氮肥增效剂、制备方法及应用 - Google Patents

一种氮肥增效剂、制备方法及应用 Download PDF

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WO2023142473A1
WO2023142473A1 PCT/CN2022/115206 CN2022115206W WO2023142473A1 WO 2023142473 A1 WO2023142473 A1 WO 2023142473A1 CN 2022115206 W CN2022115206 W CN 2022115206W WO 2023142473 A1 WO2023142473 A1 WO 2023142473A1
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nitrogen fertilizer
synergist
parts
nitrogen
fertilizer synergist
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PCT/CN2022/115206
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French (fr)
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石岩
李亚君
曹文芹
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青岛农业大学
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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
    • C05G3/40—Mixtures of one or more fertilisers with additives not having a specially fertilising activity for affecting fertiliser dosage or release rate; for affecting solubility
    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05C—NITROGENOUS FERTILISERS
    • C05C9/00—Fertilisers containing urea or urea compounds
    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05C—NITROGENOUS FERTILISERS
    • C05C9/00—Fertilisers containing urea or urea compounds
    • C05C9/005—Post-treatment
    • 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
    • C05G3/80—Soil conditioners
    • 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
    • C05G5/00—Fertilisers characterised by their form
    • C05G5/10—Solid or semi-solid fertilisers, e.g. powders
    • C05G5/12—Granules or flakes
    • 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
    • C05G5/00—Fertilisers characterised by their form
    • C05G5/30—Layered or coated, e.g. dust-preventing coatings
    • C05G5/37—Layered or coated, e.g. dust-preventing coatings layered or coated with a polymer
    • 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
    • C05G5/00—Fertilisers characterised by their form
    • C05G5/30—Layered or coated, e.g. dust-preventing coatings
    • C05G5/38—Layered or coated, e.g. dust-preventing coatings layered or coated with wax or resins
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P60/00—Technologies relating to agriculture, livestock or agroalimentary industries
    • Y02P60/20—Reduction of greenhouse gas [GHG] emissions in agriculture, e.g. CO2
    • Y02P60/21—Dinitrogen oxide [N2O], e.g. using aquaponics, hydroponics or efficiency measures

Definitions

  • the invention belongs to the technical field of fertilizers, and in particular relates to a nitrogen fertilizer synergist, a preparation method and an application.
  • nitrogen is an important component of biological macromolecules in plants, such as proteins, nucleic acids, chlorophyll and some hormones.
  • Various physiological processes such as reduction, transport and metabolism of nitrogen absorbed by crops are coordinated with protein metabolism and carbon metabolism to form the basic process of plant life activities.
  • Appropriately increasing nitrogen application within a certain range can improve crop nitrogen utilization rate, regulate the photosynthetic capacity of crop leaves, promote the accumulation of photosynthetic material in the aboveground, and then increase crop yield and dry matter accumulation.
  • Urea is the nitrogen fertilizer with the highest nitrogen content and is suitable for a variety of soils and plants. It has little damage to the soil and is a chemical nitrogen fertilizer that is currently used in large quantities.
  • Nitrogen fertilizer enters the environment in the form of NH 4 + , NO 3- , NH 3 , N 2 O and other forms and is lost, resulting in a decrease in the use efficiency of nitrogen fertilizer.
  • Such as slowing down or controlling the rate of urea dissolution by physical and chemical methods including resin-coated urea, sulfur-coated urea, urea-formaldehyde fertilizer, etc. (patent 200510026172.7, 200510136749.X); or adding urease inhibitors, nitrification inhibitors, etc., through Chemical, biochemical and other methods inhibit or regulate the rate of urea conversion. Because the nutrient release rate of coated fertilizers is easily affected by external environmental factors, it is difficult to control, and the controlled release effect is poor.
  • the slow and controlled release effect is mainly limited by the coating material; Weak inhibitory effect, but there are not many varieties that can be used in production practice and large-scale application, including the dominant inhibitors at home and abroad such as DCD, DMPP, NBPT, etc. These inhibitors have many problems that are difficult to overcome The disadvantages include short action time, great influence by temperature, high pressurization pressure, easy volatilization, can not be added to solid fertilizer, large dosage and high cost.
  • patent 202011455959.6 uses crude proanthocyanidins as raw material, adding urease inhibitors and nitrification inhibitors , nitrogen stabilizer, carrier and filler to produce a nitrogen fertilizer synergist containing plant-derived denitrification inhibitors, in which the addition of urease inhibitors and nitrification inhibitors requires complex procedures to ensure their stability; and the use of The combined synergistic approach increases the application cost, and its synergistic effect is not easy to control.
  • patent 201710594389.0 discloses a nitrogen-fixing and phosphorus-fixing high-efficiency biological fertilizer that uses itaconic acid to improve crop yields, including nitrogen-fixing fertilizers, phosphorus-fixing fertilizers, and synergistic fertilizers.
  • the synergist is composed of iron sulfate, phosphate rock powder, calcium lignosulfonate, and potassium humate, and the nitrogen-fixing fertilizer, phosphate-fixing fertilizer, and synergist are applied sequentially during fertilization, making and applying complex and difficult to popularize.
  • the combination of synergists and fertilizers can save labor costs, but the existing synergists have problems such as being easily affected by the environment, easy to be lost, and have a short action time.
  • the synergist can ensure its continuous effect during the crop growth period; during the preparation process of the synergist, the raw material of the synergist is guaranteed to be free from the influence of the fertilizer and the preparation process, which effectively saves the preparation cost and makes the synergist easy to popularize and use; at the same time, the synergist
  • the raw materials of synergists should be safe and environmentally friendly to ensure that they are harmless to the environment; in short, efficient, safe, and stable synergists can effectively improve the utilization rate of nitrogen fertilizers, reduce nitrogen loss, save agricultural production costs, and increase agricultural production benefits.
  • the disclosed embodiments of the present invention provide a nitrogen fertilizer synergist, a preparation method and an application. Described technical scheme is as follows:
  • a nitrogen fertilizer synergist is calculated in parts by weight, consisting of 15 to 20 parts of polyaspartic acid, 10 to 15 parts of 2-methylene succinic anhydride, Composed of 5-7.5 parts of acrylamide, 0.2-0.6 parts of potassium persulfate, and 800-1200 parts of distilled water.
  • the active ingredient of the nitrogen fertilizer synergist is polyaspartic acid; the film-forming agent of the nitrogen fertilizer synergist is 2-methylene succinic anhydride, acrylamide; the nitrogen fertilizer synergist
  • the initiator of the agent is potassium persulfate.
  • Another object of the present invention is to provide a kind of preparation method of the nitrogen fertilizer synergist of applying described nitrogen fertilizer synergist, the preparation method of described nitrogen fertilizer synergist comprises:
  • Each component of the raw material is weighed according to the weight part, and the dissolution reaction is carried out in the reaction kettle, and the mixed solution is fully mixed by a constant temperature vibrator to obtain the nitrogen fertilizer synergist.
  • preparation method of described nitrogen fertilizer synergist comprises the following steps:
  • Step 1 adding acrylamide, 2-methylene succinic anhydride, distilled water and potassium persulfate into the reaction kettle and stirring for reaction, and preparing a mixed aqueous solution of acrylamide and 2-methylene succinic anhydride;
  • Step 2 after cooling to room temperature, continue to slowly add polyaspartic acid to the mixed aqueous solution according to the ratio of parts by weight, and stir at room temperature to obtain a mixed solution;
  • Step 3 Pour the mixed solution into a constant temperature shaker and mix thoroughly to obtain a nitrogen fertilizer synergist.
  • acrylamide, 2-methylene succinic anhydride, distilled water and initiator potassium persulfate are added to the reactor in a ratio of 1:2:80:0.1 in parts by weight.
  • the reaction temperature in the step 1 is controlled at 30-80° C., and the reaction time is 15-20 minutes.
  • polyaspartic acid is slowly added according to the weight ratio of acrylamide to polyaspartic acid of 0.75:1, and the speed of adding polyaspartic acid is 0.1-0.3L /s, the stirring time is 15-20 min, and the stirring temperature is 18-25°C.
  • the vibration frequency of the thermostatic vibrator in the third step is 300 rpm, and the vibration time is 10-20 minutes.
  • Another object of the present invention is to provide an application of the nitrogen fertilizer synergist in fertilizer preparation.
  • the fertilizer is nitrogen fertilizer or compound fertilizer.
  • the application method of the nitrogen fertilizer synergist in fertilizer preparation comprises:
  • the nitrogen fertilizer synergist solution is added to nitrogen fertilizer or compound fertilizer by high-pressure spraying method during preparation;
  • the ratio of the synergist to the fertilizer is 1:30
  • the spray pressure is 50-75 MPa
  • the spray time is 5-15 minutes
  • the spray temperature is 10-40°C.
  • the nitrogen fertilizer synergist provided by the present invention has a simple manufacturing process, high cost-effective raw materials, and is easy to be popularized and used on a large scale.
  • the active ingredient polyaspartic acid of the nitrogen fertilizer synergist of the present invention has good ion adsorption and biodegradability, and can be slowly degraded; it is coated on the surface of fertilizer particles after being copolymerized with 2-methylene succinic anhydride and acrylamide , can form a protective film, reduce the volatilization of nitrogen fertilizer and the leaching and runoff loss of nitrogen fertilizer, and have the effect of slow release of fertilizer, so that crops can fully absorb and utilize nitrogen nutrients during the growth period, so as to promote crop growth and development and increase yield and fertilizer use efficiency purposes.
  • the nitrogen fertilizer synergist of the present invention as a synergist for regulating and controlling soil nitrogen conversion, is applied in combination with fertilizers, and compared with existing slow-release fertilizers, it has the following advantages:
  • the invention is a preparation method of a nitrogen fertilizer synergist developed aiming at the problem of low nitrogen fertilizer utilization efficiency, which solves the problems of nitrogen fertilizer volatilization, nitrogen fertilizer leaching and runoff loss, and the like.
  • the active ingredient of the nitrogen fertilizer synergist, polyaspartic acid is an amino acid polymer, which contains a large number of carboxyl and amide groups.
  • the exchange and adsorption of nutrient ions in the soil is much higher than the adsorption of soil particles to nutrient ions, which can increase the persistence of nitrogen in the soil, strengthen the absorption of nitrogen by crops, and reduce nitrogen loss , increase soil fertility.
  • the nitrogen fertilizer synergist film-forming agent 2-methylene succinic anhydride contains active functional groups such as carbon-carbon unsaturated double bonds and anhydride groups in its molecule, and is an important polymerized monomer for the production of polymer materials; the nitrogen fertilizer
  • the synergist initiator potassium persulfate undergoes covalent bond homolysis under the action of heat or light to generate two free radicals, which can initiate a polymerization reaction.
  • the film-forming agent acrylamide and 2-methylene succinic anhydride are used
  • the copolymer obtained by the copolymerization of the linked monomer is mixed with polyaspartic acid to coat the fertilizer after cross-linking, so that a protective film is formed on the outside of the fertilizer particles, and urea is gradually released through slow degradation, reducing the waste of urea.
  • the nitrogen loss can be reduced by about 5% to 7% cumulatively.
  • the manufacturing process is simple and easy to use.
  • the nitrogen fertilizer synergist of the present invention utilizes the properties of the material itself to polymerize to form a film, without the need for special matching fertilizer processing technology, and can be used in agricultural production by adding the nitrogen fertilizer synergist solution to nitrogen fertilizer or compound fertilizer by using a high-pressure spraying method.
  • the contact area between polyaspartic acid and raw materials is reduced, and factors such as high temperature, damp heat, and slight negative pressure during the granulation process are avoided Effects on the molecular structure of polyaspartic acid.
  • Spraying the nitrogen fertilizer synergist of the present invention on the surface of the fertilizer can be used for agricultural production, and the dosage is small, replacing other inhibitors and reducing the fertilizer cost.
  • Fig. 1 is a flow chart of the preparation method of the nitrogen fertilizer synergist provided by the embodiment of the present invention.
  • Fig. 2 is a comparison diagram between the synergistic nitrogen fertilizer (urea) and ordinary urea prepared by spraying the nitrogen fertilizer synergist prepared by the present invention on the surface of urea and air-drying provided by the embodiment of the present invention.
  • the present invention provides a nitrogen fertilizer synergist, its preparation method and application.
  • the present invention will be described in detail below in conjunction with the accompanying drawings.
  • the purpose of the present invention is to provide a method for preparing a nitrogen fertilizer synergist, which can reduce the volatilization of nitrogen fertilizer and the leaching and runoff loss of nitrogen fertilizer, and play a role in the slow release of fertilizer. Effect.
  • the nitrogen fertilizer synergist provided by the embodiments of the present invention consists of 15-20 parts of polyaspartic acid, 10-15 parts of 2-methylene succinic anhydride, 5-7.5 parts of acrylamide, potassium persulfate 0.2-0.6 parts, 800-1200 parts of distilled water.
  • the preparation method of the nitrogen fertilizer synergist that the embodiment of the present invention provides comprises the following steps:
  • the nitrogen fertilizer synergist prepared by the invention can be used for production after being sprayed on the surface of urea and air-dried.
  • Fig. 2 is a comparison diagram between the synergistic nitrogen fertilizer (urea) and common urea made after the nitrogen fertilizer synergist of the present invention is sprayed on the surface of urea and air-dried. As shown in Figure 2, the synergist forms a protective film on the surface of urea granules.
  • the nitrogen fertilizer synergist prepared according to the raw materials in Example 1 was sprayed on the surface of urea to obtain synergistic urea, and the obtained synergistic urea was used for the wheat growth and development test.
  • Three treatments were set up in the experiment, which were control treatment: urea 50kg/667m 2 without synergist; treatment 1: synergistic urea 50kg/667m 2 with synergist; treatment 2: synergistic urea 37.5kg/667m 2 , plus synergist, wheat was sown on October 23, with a sowing rate of 12kg per 667m 2 .
  • Nitrogen is a component of chlorophyll. It can be seen from Table 3 that the chlorophyll content of wheat flag leaves in treatment and treatment 2 is more than that of nitrogen fertilizer alone, indicating that the addition of synergists can maintain a high chlorophyll content in wheat, which is beneficial to wheat growth.
  • adding synergists when applying urea is more conducive to the growth and development of wheat, and under certain urea reduction conditions, it can still maintain a high yield of wheat, indicating that synergists can promote wheat to fully absorb and utilize nitrogen Nutrition, reduce nitrogen loss, and its effect has the characteristics of synergistic, long-term and stable effect.
  • the nitrogen fertilizer synergist prepared according to the raw materials in Example 1 was sprayed on the surface of the fertilizer to obtain a synergistic compound fertilizer, which was used in a corn growth and development test, and the tested variety was Qiule 218.
  • Corn is sown in mid-to-late June, with 4,800 plants per mu, with a large row spacing of 80 cm, a small row spacing of 50 cm, and a plant spacing of 18 cm.
  • all fertilizers are used as base fertilizers for one-time fertilization, and no topdressing operation is performed in the later stage. Irrigation measures are not used during the corn growth period, and only natural precipitation is relied on.
  • T1 was higher than CK in terms of panicle number, grain number per panicle and thousand-grain weight.
  • the yield of T1 was 8.55% higher than that of CK.
  • Wheat morphological indicators Take 10*3 wheat fresh samples after wheat flowering, measure the plant height and the number of leaves on the main stem after flowering; take 10*3 wheat samples after the wheat matures, measure the ear length, the internode below the ear long.
  • Chlorophyll content of wheat leaves From 9 to 11 in the morning when the weather is clear and windy, the flag leaves of wheat main stem functional leaves were randomly selected to measure the chlorophyll content of field wheat within 0 to 35 days after flowering, and the chlorophyll content was measured using SPAD-502 (Japan Production) Portable Chlorophyll Measuring Instrument, the average value of multiple measurements is taken.
  • the test results are shown in Tables 6-9.
  • the morphological indicators of wheat showed that treatment 1 and treatment 2 were better than the control; dry matter accumulation in aboveground parts, chlorophyll content in leaves and yield showed that treatment 1> treatment 2> control. That is to say, under the condition of using the same amount of urea, adding a synergist to make synergistic urea, the growth of wheat is more advantageous, and under the treatment of reducing urea by 75% and adding a synergist, the performance of various indicators of wheat is also better than that of single Apply urea treatment.
  • Corn is sown in mid-to-late June, with 4,800 plants per mu, with a large row spacing of 80 cm, a small row spacing of 50 cm, and a plant spacing of 18 cm.
  • all fertilizers are used as base fertilizers for one-time fertilization, and no topdressing operation is performed in the later stage. Irrigation measures are not used during the corn growth period, and only natural precipitation is relied on.
  • T1 is higher than CK in terms of panicle number, grain number per panicle and 1000-grain weight, and the yield of T1 is 8.55% higher than that of CK.
  • the synergist combined with urea is beneficial to the absorption and utilization of nitrogen by corn, promotes its growth and development, and increases corn yield.

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Abstract

本发明属于肥料技术领域，公开了一种氮肥增效剂、制备方法及应用，所述氮肥增效剂按照重量份数计由聚天门冬氨酸15～20份、2-亚甲基丁二酸酐10～15份、丙烯酰胺5～7.5份、过硫酸钾0.2～0.6份、蒸馏水800～1200份组成；所述氮肥增效剂的制备方法包括：将原料各组分按重量份称量好后在反应釜中进行溶解反应，混合液经恒温震动器充分混匀得氮肥增效剂。本发明氮肥增效剂的有效成分聚天门冬氨酸具有良好的离子吸附性和生物可降解性；与2-亚甲基丁二酸酐、丙烯酰胺共聚后包裹在肥料颗粒表面形成保护膜，能够减少氮肥的挥发和氮肥的淋溶与径流损失，起到肥料缓释的效果，促进作物的生长发育，提高产量和肥料利用效率。

Description

一种氮肥增效剂、制备方法及应用 技术领域
本发明属于肥料技术领域，尤其涉及一种氮肥增效剂、制备方法及应用。
背景技术
目前，氮素是植物体内生物大分子的重要组成成分，如蛋白质，核酸，叶绿素和部分激素。作物吸收的氮素所经过的还原、转运和代谢等各种生理过程，与蛋白质代谢和碳代谢相协调，形成植物生命活动的基本过程在一定范围内适当增加施氮量能提高作物氮素利用率，调控作物叶片光合能力，促进地上部光合物质的积累，进而提高作物产量、干物质积累量。尿素是氮量最高的氮肥，适用于各种土壤和植物。对土壤的破坏作用小，是目前使用量较大的一种化学氮肥，但尿素在土壤中分解较快，在土壤中易流失，施入土壤的尿素，除被作物吸收和土壤固定外，其余氮肥以NH 4 +、NO 3-、NH 3、N 2O等形态进入环境而流失，造成氮肥利用效率降低。
研究表明，氮肥利用率为28％～41％，中国大田作物氮肥平均利用率仅有30％，大部分氮肥经氨挥发、反硝化作用、地表径流和地下渗漏等途径损失并进入环境中。农业生产中，片面追求高产而盲目增施氮肥不仅降低作物氮素利用率，造成资源浪费、成本增加，还会引导致土壤污染、地下水硝态氮含量超标、大气中氧化亚氮排放量增加、 江河湖泊水体富营养化等一系列的环境污染问题，严重威胁农业的可持续发展和人类的健康；因此，采取措施提高氮肥的利用率，对环境保护和作物高效安全生产具有重要意义。
目前，提高氮素利用率、降低肥料损失、控制环境污染的方法有很多，包括测土配方施肥；合理追施氮肥；有机肥代替部分化肥；精准施肥；秸秆还田，增加土壤有机质含量，改变土壤结构等，虽能有效提高氮素利用率和产量，弥补尿素因氨挥发、径流、淋溶等原因造成的缺失，但势必会增加劳动成本。为满足开发能耗低、成本低、效果好等需求，肥料增值技术和发展增值肥料受到国内外新型肥料研究的的青睐。如用物理、化学的方法减缓或控制尿素溶出的速率，包括树脂包衣尿素、硫包衣尿素、脲醛肥料等(专利200510026172.7，200510136749.X)；或添加脲酶抑制剂、硝化抑制剂等，通过化学、生化等方法抑制或调控尿素转化的速率。包膜肥料由于其养分释放速度易受外界环境因素影响，难以控制，控释效果较差，缓控释效果主要受包膜材料限制；迄今为止，已发现有数百种化合物显示了或强或弱的抑制效应，但是真正能够用于生产实践并进行大规模推广应用的品种并不多，包括国内外居主导地位的抑制剂DCD、DMPP、NBPT等，这些抑制剂其自身存在着许多难以克服的缺点，包括作用时间短，受温度影响大，增气压高，易挥发，无法添加到固体肥料中，用量大，成本高，如专利202011455959.6以原花青素粗品为原料，添加脲酶抑制剂、硝化抑制剂、氮素稳定剂、载体和填充剂制作了一种含植物源反硝化抑制剂的氮肥增效剂，其中脲酶抑制剂、硝化抑制剂的添加 则需要以复杂工序以保证其稳定性；而采用组合协同增效的方式则提高了应用成本，且其协同效应不易控制，如专利201710594389.0公开了一种利用衣康酸提高作物产量的固氮固磷高效生物肥料，包括固氮肥、固磷肥和增效剂，采用衣康酸、马来酸酐和乙酸酐分别在过硫酸钾和叔丁基过氧化氢的引发条件下聚合，所得聚合物再与常规氮肥和磷肥混合均匀，可起到较好的固氮、固磷效果，同时，对增效剂的原料及配比进行选择，使其能与固氮固磷肥相辅相成，协同配合，更多地提供农作物生长吸收所需的磷、氮等营养元素，然而其增效剂由硫酸铁、磷矿粉、木质素磺酸钙、腐殖酸钾组成，且固氮肥、固磷肥和增效剂在施肥时前后依次施加，制作和施用复杂，不易推广。
因此，高效低毒、性能稳定的新型增效剂材料的筛选和协同增效组合技术仍然是国内外科学家关注的热点，具有很重要的农学和生态学意义。
通过上述分析，现有技术存在的问题及缺陷为：
(1)采用测土配方施肥、合理追施氮肥、精准施肥、秸秆还田等方法，虽能有效提高氮素利用率，减少氮素损失，但会增加劳动成本。
(2)现有的包膜肥料由于其养分释放速度易受外界环境因素影响，难以控制，控释效果较差，缓控释效果主要受包膜材料限制。
(3)现有真正能够用于生产实践并进行大规模推广应用的品种并不多，且现有抑制剂的作用时间短，受温度影响大，增气压高，易挥发，无法添加到固体肥料中，用量大，成本高。
解决以上问题及缺陷的难度为：
(1)所选增效剂是否能够发挥作用；是否性能稳定，是否易受外界环境影响，是否能够在作物生育期内持续作用；是否安全环保。
(2)所选增效剂是否能够均匀整合到肥料中或喷涂于肥料表面；其性能是否易受肥料影响。
(3)所选增效剂原材料是否易得；制造成本是否可控；在制备过程中是否易损失。
解决以上问题及缺陷的意义为：增效剂与肥料配施能够节约劳动成本，但现有增效剂存在易受环境影响、易损失、作用时间短等问题，因此研究制备性能稳定的增效剂能够保证其在作物生育期内持续作用；在增效剂制备过程中，保证增效剂原材料免受肥料和制备工艺的影响，有效节约制备成本，使增效剂易于推广使用；同时，增效剂原材料应安全环保，确保其对环境无害；总之，高效、安全、性能稳定的增效剂能够有效提高氮肥利用率，减少氮素损失，节约农业生产成本，增加农业生产效益。
发明内容
为克服相关技术中存在的氮肥利用效率低的问题，本发明公开实施例提供了一种氮肥增效剂、制备方法及应用。所述技术方案如下：
本发明是这样实现的，一种氮肥增效剂，所述氮肥增效剂按照重量份数计，由聚天门冬氨酸15～20份、2-亚甲基丁二酸酐10～15份、丙烯酰胺5～7.5份、过硫酸钾0.2～0.6份、蒸馏水800～1200份组成。
在一个实施例中，所述氮肥增效剂的有效成分为聚天门冬氨酸；所述氮肥增效剂的成膜剂为2-亚甲基丁二酸酐、丙烯酰胺；所述氮肥增效剂的引发剂为过硫酸钾。
本发明的另一目的在于提供一种应用所述的氮肥增效剂的氮肥增效剂的制备方法，所述氮肥增效剂的制备方法包括：
将原料各组分按照重量份称量好，在反应釜中进行溶解反应，混合液经恒温震动器充分混匀，得到氮肥增效剂。
进一步，所述氮肥增效剂的制备方法包括以下步骤：
步骤一，将丙烯酰胺、2-亚甲基丁二酸酐、蒸馏水及过硫酸钾加入反应釜中搅拌进行反应，配制得到丙烯酰胺、2-亚甲基丁二酸酐混合水溶液；
步骤二，待冷却至室温后，继续向混合水溶液中按照重量份数比缓慢添加聚天门冬氨酸，进行常温搅拌，得到混合液；
步骤三，将混合液倒入恒温震动器充分混匀，得氮肥增效剂。
在一个实施例中，所述步骤一中，将丙烯酰胺、2-亚甲基丁二酸酐、蒸馏水及引发剂过硫酸钾按照重量份数配比1：2：80：0.1加入反应釜。
在一个实施例中，所述步骤一中的反应温度控制在30～80℃，所述反应时间为15～20min。
在一个实施例中，所述步骤二中，按照丙烯酰胺与聚天门冬氨酸重量份数比0.75：1缓慢添加聚天门冬氨酸，所述添加聚天门冬氨酸速度为0.1～0.3L/s，所述搅拌时间为15～20min，所述搅拌温度为 18～25℃。
在一个实施例中，所述步骤三中的恒温震动器震动频率为300rpm，所述震动时间为10～20min。
本发明的另一目的在于提供一种所述的氮肥增效剂在肥料制备中的应用。
在一个实施例中，所述肥料为氮肥或复合肥。
在一个实施例中，所述氮肥增效剂在肥料制备中的应用方法包括：
在制备时采用高压喷淋法将所述氮肥增效剂溶液加入氮肥或复合肥中；
其中，所述增效剂与肥料比例为1：30，所述喷淋压力为50～75MPa，所述喷淋时间为5～15min，所述喷淋温度为10～40℃。
结合上述的所有技术方案，本发明所具备的优点及积极效果为：本发明提供的氮肥增效剂制造工艺简单，原料性价比高，容易大面积推广使用。本发明的氮肥增效剂的有效成分聚天门冬氨酸具有良好的离子吸附性和生物可降解性，可缓慢降解；与2-亚甲基丁二酸酐、丙烯酰胺共聚后包裹在肥料颗粒表面，可形成保护膜，减少氮肥的挥发和氮肥的淋溶与径流损失，起到肥料缓释的效果，使作物能够在生长期内充分吸收利用氮素营养，从而达到促进作物生长发育，提高产量和肥料利用效率的目的。
本发明的氮肥增效剂作为调控土壤氮素转化的增效剂，与肥料配施，同现有的缓控释肥相比，具有以下优点：
1.应用效果好。本发明是针对氮肥利用效率低的问题而研制的一种氮肥增效剂的制备方法，解决氮肥的挥发和氮肥的淋溶与径流损失等问题。所述氮肥增效剂有效成分聚天门冬氨酸是一种氨基酸类聚合物，含有大量的羧基和酰胺基团，自身带有正、负两类电荷，可吸收和富集土壤中对植物生长有利的元素，对土壤中养分离子的交换吸附力远远高于土壤颗粒自身对养分离子的吸附力，能增加土壤中氮素的持效性，强化作物对氮素的吸收，减少氮素损失，增加土壤的肥力。所述氮肥增效剂成膜剂2-亚甲基丁二酸酐，其分子中含有碳—碳不饱和双键以及酐基等活性官能团，是高分子材料生产的重要聚合单体；所述氮肥增效剂引发剂过硫酸钾在热或光的作用下发生共价键均裂而生成两个自由基，能够引发聚合反应，将成膜剂丙烯酰胺、2-亚甲基丁二酸酐作为交联性单体共聚得到的共聚物与聚天门冬氨酸混合交联后对化肥进行包衣，使肥料颗粒外形成保护膜，通过缓慢的降解逐渐释放尿素，减少尿素的浪费。在如小麦、玉米等大田作物的生育期内，可累积减少约5％～7％的氮素损失。
2.制造工艺简单，使用方便。本发明的氮肥增效剂利用材料自身的性质聚合成膜，无需特殊配套肥料加工工艺，采用高压喷淋法将所述氮肥增效剂溶液加入氮肥或复合肥中即可用于农业生产。相比于将聚天门冬氨酸与原料混合后进入生产系统进行造粒，减少了聚天门冬氨酸与原材料的接触面积，同时避免了造粒过程中的高温、湿热、微负压等因素对聚天门冬氨酸分子结构的影响。
3.成本低，用量少。将本发明的氮肥增效剂喷涂于肥料表面即 可用于农业生产，用量少，代替其他抑制剂，降低肥料成本。
当理解的是，以上的一般描述和后文的细节描述仅是示例性和解释性的，并不能限制本发明的公开。
附图说明
此处的附图被并入说明书中并构成本说明书的一部分，示出了符合本公开的实施例，并与说明书一起用于解释本公开的原理。
图1是本发明实施例提供的氮肥增效剂的制备方法流程图。
图2是本发明实施例提供的本发明制备的氮肥增效剂喷涂于尿素表面风干后制成的增效氮肥(尿素)与普通尿素的对比图。
具体实施方式
为使本发明的上述目的、特征和优点能够更加明显易懂，下面结合附图对本发明的具体实施方式做详细的说明。在下面的描述中阐述了很多具体细节以便于充分理解本发明。但是本发明能够以很多不同于在此描述的其他方式来实施，本领域技术人员可以在不违背本发明内涵的情况下做类似改进，因此本发明不受下面公开的具体实施的限制。
针对现有技术存在的问题，本发明提供了一种氮肥增效剂、制备方法及应用，下面结合附图对本发明作详细的描述。
针对现有技术中存在的氮肥利用效率低的问题等问题，本发明的目的在于提供一种氮肥增效剂的制备方法，减少氮肥的挥发和氮肥的 淋溶与径流损失，起到肥料缓释的效果。
本发明实施例提供的氮肥增效剂按照重量份数计，由聚天门冬氨酸15～20份、2-亚甲基丁二酸酐10～15份、丙烯酰胺5～7.5份、过硫酸钾0.2～0.6份、蒸馏水800～1200份组成。
如图1所示，本发明实施例提供的氮肥增效剂的制备方法包括以下步骤：
S101，将丙烯酰胺、2-亚甲基丁二酸酐、蒸馏水及引发剂过硫酸钾加入反应釜中搅拌进行反应，配制得到丙烯酰胺、2-亚甲基丁二酸酐混合水溶液；
S102，待冷却至室温后，继续向混合水溶液中按照重量份数比缓慢添加聚天门冬氨酸，进行常温搅拌，得到混合液；
S103，将混合液倒入恒温震动器充分混匀，得氮肥增效剂。
将本发明制备得到的氮肥增效剂喷涂于尿素表面经风干即可用于生产。图2是本发明氮肥增效剂喷涂于尿素表面风干后制成的增效氮肥(尿素)与普通尿素的对比图。如图2所示，增效剂在尿素颗粒表面形成一层保护膜。
下面结合具体实施例对本发明的技术方案作进一步描述。
实施例1
本发明实施例提供的氮肥增效剂的原料各组分按照重量份组成如下：
聚天门冬氨酸8～10份、2-亚甲基丁二酸酐12～15份、丙烯酰胺6～7.5份、过硫酸钾0.2～0.6份、蒸馏水800～1200份。
本发明实施例提供的氮肥增效剂的制备方法如下：
将丙烯酰胺、2-亚甲基丁二酸酐、蒸馏水及引发剂过硫酸钾按照重量份数配比1：2：80：0.1加入反应釜中搅拌，控制温度在30～80℃，反应15～20分钟，配制成丙烯酰胺、2-亚甲基丁二酸酐混合水溶液。冷却至室温后按照丙烯酰胺与聚天门冬氨酸重量份数比0.75：1缓慢添加聚天门冬氨酸，进行常温搅拌。将混合液倒入恒温震动器充分混匀即得氮肥增效剂溶液。
按照实施例1的原料配制的氮肥增效剂喷涂于尿素表面，即得增效尿素，将所得增效尿素用于小麦生长发育试验。试验设置3个处理，分别为对照处理:尿素50kg/667m 2，不加增效剂；处理1：增效尿素50kg/667m 2，加增效剂；处理2：增效尿素37.5kg/667m 2，加增效剂，小麦于10月23日播种，每667m 2播量为12kg。试验采用不完全随机区组设计，每个处理面积10*30＝300m 2，每个处理设3次重复。此外，所有肥料均作为底肥进行一次性施肥，生育期间亦不采用灌溉措施，仅依靠自然降水。分别于小麦开花后的0～35d隔7d取样，测定相应指标。
表1不同处理下小麦形态指标
Figure PCTCN2022115206-appb-000001
由表1可知，在施用等量尿素的条件下，添加增效剂制成增效尿素施用，小麦的形态指标较为优势，而在尿素减量75％、添加增效剂 的处理下，小麦的形态指标表现也优于单施尿素处理，说明增效剂对小麦吸收利用尿素中的氮素营养具有补充效益。
表2不同处理下小麦地上部干物质积累量(g/株)
处理 开花期 花后7d 花后14d 花后21d 花后28d 花后35d
对照 24.60 29.90 33.77 36.76 43.44 48.00
处理1 33.35 38.39 41.88 50.78 53.69 56.99
处理2 27.17 34.23 37.54 43.45 51.22 53.33
由表2可知，处理1与处理2小麦地上部干物质积累量多于对照处理，说明添加增效剂后施氮肥效果优于单施氮肥，且在氮肥减量的情况下仍能使小麦保持较高的干物质积累量。
表3不同处理下小麦旗叶叶绿素含量
处理 开花期 花后7d 花后14d 花后21d 花后28d 花后35d
对照 58.94 57.66 55.07 48.61 33.36 48.00
处理1 66.33 65.35 59.88 51.77 35.94 56.99
处理2 62.47 60.89 57.70 50.22 34.23 53.33
氮素是叶绿素的组成成分，由表3可知，处理与处理2小麦旗叶的叶绿素含量多于单施氮肥，说明添加增效剂能够使小麦保持较高的叶绿素含量，利于小麦生长。
表4不同处理对小麦产量的影响
处理 穗数(10 4/667m 2) 穗粒数(个/穗) 千粒重(g) 产量(kg/667m 2)
对照 39.54 33.55 38.29 507.94
处理1 40.76 34.19 40.03 557.85
处理2 40.11 33.69 39.75 537.14
由表4可知，施用添加增效剂的增效尿素可使小麦群体的亩穗数、穗粒数、千粒重保持在较高水平，最终产量优于单施尿素处理。
综上，在施用尿素时添加增效剂更利于小麦生长发育，且在一定的尿素减量条件下，仍能使小麦保持较高的产量，说明增效剂能够促 进小麦充分吸收与利用氮素营养、降低氮素损失，且其作用具有增效性、长效性和稳效性的特点。
实施例2
按照实施例1的原料配制的氮肥增效剂喷涂于肥料表面，即得增效复合肥，将其用于玉米生长发育试验，供试品种为秋乐218。试验设置2个处理，分别为对照处理(CK)：复合肥(氮：磷：钾＝20：15：10)50kg/667m 2，不加增效剂；处理(T1)：增效复合肥(氮：磷：钾＝20：15：10)50kg/667m 2。玉米于6月中下旬播种，每亩播种4800株，大行距80cm、小行距50cm，株距18cm。试验采用不完全随机区组设计，每个处理面积0.8*130＝114m 2，每个处理设3次重复。此外，所有肥料均作为底肥进行一次性地施肥，后期不进行任何的追肥操作，玉米生育期间亦不采用灌溉措施，仅依靠自然降水。
表5不同处理对玉米产量的影响
处理 穗数(穗/667m 2) 穗粒数(粒/穗) 百粒重(g) 产量(kg/667m 2)
CK 4759 309 40.17 590.71
T1 4775 325 41.32 641.23
在穗数、穗粒数和千粒重方面，T1高于CK。T1比CK增产了8.55％。
下面结合具体实验对本发明的技术效果作进一步描述。
试验1
一、试验设计
试验设置3个处理，分别为对照处理：尿素50kg/667m 2，不加增效剂；处理1：增效尿素50kg/667m 2，加增效剂；处理2：增效尿素37.5kg/667m 2，加增效剂。试验采用不完全随机区组设计，每个处理 面积10*30＝300m 2，每个处理设3次重复。
小麦于10月23日播种，每667m 2播量为12kg。所有肥料均作为底肥进行一次性施肥，生育期间不采用灌溉措施，仅依靠自然降水。
二、测定项目与方法
1、小麦形态指标：在小麦开花后取小麦新鲜样品10*3株，测定株高、花后主茎叶片数；在小麦成熟后取样品10*3株，测定穗长、穗下节间长。
2、地上部干物质积累量：在小麦开花后0～35d内每隔7d取地上部鲜样，将鲜样先杀青再烘干，称重。
3、小麦叶片叶绿素含量：天气晴朗少风的上午9至11时，在大田小麦在开花后的0～35d内隔7d随机选用小麦主茎功能叶片旗叶测定叶绿素含量，使用SPAD-502(日本生产)便携式叶绿素测定仪，多次测定取平均值。
4、小麦产量：各处理分小区内选1m 2的完整小麦植株分别重复3次，进行成穗数检查，再计算公顷穗数。自然风干后进行脱粒，考种测定穗粒数和千粒重，并计算产量
三、结果与分析
表6不同处理下小麦形态指标
Figure PCTCN2022115206-appb-000002
Figure PCTCN2022115206-appb-000003
表7不同处理下小麦地上部干物质积累量(g/株)
Figure PCTCN2022115206-appb-000004
表8不同处理下小麦旗叶叶绿素含量
Figure PCTCN2022115206-appb-000005
表9不同处理对小麦产量的影响
Figure PCTCN2022115206-appb-000006
试验结果如表6～9所示，小麦形态指标表现为处理1、处理2优 于对照；地上部干物质积累量、叶片叶绿素含量及产量表现为处理1>处理2>对照。即在施用等量尿素的条件下，添加增效剂制成增效尿素施用，小麦长势较为优势，而在尿素减量75％、添加增效剂的处理下，小麦各指标表现也优于单施尿素处理。
四、结论
综合以上分析可知，增效剂配施尿素有利于小麦对氮素的吸收，从而促进小麦生长，增加产量；且在尿素减量的情况下，小麦长势及最终产量仍能维持在较高水平。
试验2
一、试验设计
供试玉米品种为秋乐218。试验设置2个处理，分别为对照处理(CK)：复合肥(氮：磷：钾＝20：15：10)50kg/667m 2，不加增效剂；处理(T1)：增效复合肥(氮：磷：钾＝20：15：10)50kg/667m 2。
玉米于6月中下旬播种，每亩播种4800株，大行距80cm、小行距50cm，株距18cm。试验采用不完全随机区组设计，每个处理面积0.8*130＝114m 2，每个处理设3次重复。此外，所有肥料均作为底肥进行一次性地施肥，后期不进行任何的追肥操作，玉米生育期间亦不采用灌溉措施，仅依靠自然降水。
二、测定项目与方法
各处理分小区内选3m 2的完整植株分别重复3次，进行成穗数检查，再计算公顷穗数。自然风干后进行脱粒，考种测定穗粒数和千粒重，并计算产量。
三、结果与分析
表10不同处理对玉米产量的影响
Figure PCTCN2022115206-appb-000007
试验结果如表10所示，在穗数、穗粒数和千粒重方面，T1高于CK，T1较CK增产了8.55％。
四、结论
增效剂配施尿素有利于玉米对氮素的吸收利用，促进其生长发育，增加玉米产量。
以上所述，仅为本发明的具体实施方式，但本发明的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明揭露的技术范围内，凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，都应涵盖在本发明的保护范围之内。

Claims (10)

  1. 一种氮肥增效剂，其特征在于，所述氮肥增效剂按照重量份数计，由聚天门冬氨酸15～20份、2-亚甲基丁二酸酐10～15份、丙烯酰胺5～7.5份、过硫酸钾0.2～0.6份、蒸馏水800～1200份组成。
  2. 如权利要求1所述氮肥增效剂，其特征在于，所述氮肥增效剂的有效成分为聚天门冬氨酸；
    所述氮肥增效剂的成膜剂为2-亚甲基丁二酸酐、丙烯酰胺；
    所述氮肥增效剂的引发剂为过硫酸钾。
  3. 一种实施如权利要求1～2任意一项所述氮肥增效剂的制备方法，其特征在于，该氮肥增效剂的制备方法包括：
    将原料各组分按照重量份称量好，在反应釜中进行溶解反应，混合液经恒温震动器充分混匀，得到氮肥增效剂。
  4. 如权利要求3所述氮肥增效剂的制备方法，其特征在于，所述氮肥增效剂的制备方法具体包括以下步骤：
    步骤一，将丙烯酰胺、2-亚甲基丁二酸酐、蒸馏水及过硫酸钾加入反应釜中搅拌进行反应，配制得到丙烯酰胺、2-亚甲基丁二酸酐混合水溶液；
    步骤二，待冷却至室温后，继续向混合水溶液中按照重量份数比缓慢添加聚天门冬氨酸，进行常温搅拌，得到混合液；
    步骤三，将混合液倒入恒温震动器充分混匀，得氮肥增效剂。
  5. 如权利要求4所述氮肥增效剂的制备方法，其特征在于，所述步骤一中，将丙烯酰胺、2-亚甲基丁二酸酐、蒸馏水及过硫酸钾按照重量份数配比1：2：80：0.1加入反应釜。
  6. 如权利要求4所述氮肥增效剂的制备方法，其特征在于，所述步骤一中的反应温度控制在30～80℃，所述反应时间为15～20min。
  7. 如权利要求4所述氮肥增效剂的制备方法，其特征在于，所述步骤二中，按照丙烯酰胺与聚天门冬氨酸重量份数比0.75：1缓慢添加聚天门冬氨酸，所述添加聚天门冬氨酸速度为0.1～0.3L/s，所述搅拌时间为15～20min，所述搅拌温度为18～25℃。
  8. 如权利要求4所述氮肥增效剂的制备方法，其特征在于，所述步骤三中的恒温震动器震动频率为300rpm，所述震动时间为10～20min。
  9. 一种如权利要求1～2任意一项所述氮肥增效剂在肥料制备中的应用，其特征在于，所述肥料为氮肥或复合肥。
  10. 如权利要求9所述氮肥增效剂在肥料制备中的应用，其特征在于，所述氮肥增效剂在肥料制备中的应用方法包括：
    在制备时采用喷淋法将所述氮肥增效剂溶液加入氮肥或复合肥中；
    其中，所述增效剂与肥料比例为1：30，所述喷淋压力为50～75MPa，所述喷淋时间为5～15min，所述喷淋温度为10～40℃。
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