WO2019075971A1 - Engrais soluble dans l'eau et procédé de préparation associé - Google Patents

Engrais soluble dans l'eau et procédé de préparation associé Download PDF

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Publication number
WO2019075971A1
WO2019075971A1 PCT/CN2018/076370 CN2018076370W WO2019075971A1 WO 2019075971 A1 WO2019075971 A1 WO 2019075971A1 CN 2018076370 W CN2018076370 W CN 2018076370W WO 2019075971 A1 WO2019075971 A1 WO 2019075971A1
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WO
WIPO (PCT)
Prior art keywords
water
titanium
soluble fertilizer
fertilizer according
gluconic acid
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PCT/CN2018/076370
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English (en)
Chinese (zh)
Inventor
家新发
付荣伟
马玲
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日正九安科技（北京）有限公司
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Publication of WO2019075971A1 publication Critical patent/WO2019075971A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05C—NITROGENOUS FERTILISERS
    • C05C11/00—Other nitrogenous fertilisers
    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05C—NITROGENOUS FERTILISERS
    • C05C3/00—Fertilisers containing other salts of ammonia or ammonia itself, e.g. gas liquor
    • 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
    • C05G5/20—Liquid fertilisers

Definitions

  • the invention relates to the field of processing of fertilizers, in particular to a water-soluble fertilizer and a preparation method thereof.
  • Titanium-containing fertilizer has been proved to be a broad-spectrum, low-use functional fertilizer, which has a good promoting effect on plant physiological activities, can enhance the absorption of various nutrients by plants, and enhance plant disease resistance and stress resistance.
  • the ability to increase crop yields and improve crop quality is therefore a promising new fertilizer variety.
  • Due to the unstable nature of the inorganic titanium salt it is easy to decompose into water-insoluble titanium dioxide under natural conditions and cannot be absorbed and utilized by plants.
  • organic chelated complex titanium fertilizers have been developed and have been applied to agricultural production. In the technical measures.
  • the organic titanium functional fertilizers that have been used include VC (ascorbic acid) titanium, titanium citrate, complex organic acids (tartaric acid, citric acid, malic acid, mandelic acid, lactic acid, etc.) complexed titanium and amine carboxyl complexing agents. (EDTA, HEDTA, EDDHA, etc.) complexes titanium and has achieved good application results.
  • the object of the present invention is to provide a water-soluble fertilizer which firstly combines gluconic acid as a ligand to complex titanium ions to form a functional fertilizer of titanium gluconate complex.
  • This type of fertilizer is non-toxic and better. It is absorbed and utilized by crops, is environmentally friendly, and the ratio of each element is more reasonable. It can improve the yield and quality of crops, and it will not cause soil compaction. It has the advantages of soil control and environmental protection, and is very suitable for crop production.
  • a second object of the present invention is to provide a preparation method using the above water-soluble fertilizer, wherein the preparation method has the advantages of close connection, simple operation, no three wastes, safety and environmental protection, and the fertilizer efficiency of the variety is realized by rational design of the whole preparation method. Improvement is worthy of widespread application.
  • the present invention provides a water-soluble fertilizer mainly composed of a titanium gluconate complex and a basic substance, wherein the titanium gluconate complex is composed of a gluconic acid substance and a titanium compound according to a coordination molar ratio (2) -5): 1 made.
  • organic titanium functional fertilizers such as VC (ascorbic acid) titanium, titanium citrate, complex organic acids (tartaric acid, citric acid, malic acid, mandelic acid, lactic acid, etc.) complex titanium, amine carboxyl network
  • VC ascorbic acid
  • complex organic acids tartaric acid, citric acid, malic acid, mandelic acid, lactic acid, etc.
  • EDTA, HEDTA, EDDHA, etc. complexes titanium and has achieved good application results.
  • titanium functional fertilizers also have a series of problems, such as poor stability, high production cost, complicated manufacturing process, poor compatibility with other fertilizers, and effective absorption of crop growth.
  • the present invention provides a water-soluble fertilizer containing a titanium gluconate complex, which is not only highly efficient and environmentally friendly, but also can be well absorbed by crops and plants, and has a wide application range. Has a wide range of promotional value.
  • the titanium gluconate complex is prepared from a gluconic acid substance and a titanium compound according to a coordination molar ratio (2-5): 1, in fact, the ligand gluconic acid can be mass-produced industrially and has been widely used in foods.
  • Additives and feed additives are ordinary glucose, and the toxicity is very low.
  • the downstream products such as gluconolactone, calcium gluconate, sodium gluconate, zinc gluconate and ferrous gluconate are recognized as food nutrition regulating additives.
  • Gluconic acid itself is easily digested and absorbed by the organism, and is also very easily degraded by nature. It can be regarded as a non-toxic, non-polluting green substance.
  • gluconic acid has not been used as a ligand to complex titanium ions to prepare titanium gluconate complex.
  • the present invention firstly uses gluconic acid as a ligand to complex titanium ions to form a complex to obtain a water-soluble fertilizer, and has achieved good fertilizer efficiency.
  • the complex formed by the gluconic acid ligand and the titanium ion has high stability, and the complex can participate in nutrient metabolism in the plant, is fully absorbed and utilized by the plant, promotes vegetative growth and reproductive growth of the plant, and can be degraded in nature. Harmless substances will not adversely affect the environment.
  • the gluconic acid substance and Ti(IV) satisfy the following relationship: 2 ⁇ (number of moles of ligand): the number of moles of Ti (IV) ⁇ 5, preferably, the gluconic acid substance and the titanium compound are coordinated
  • the molar ratio can also be 3:1, 4:1, etc., through reasonable coordination of the number of moles, so that the two can form an effective complex.
  • the titanium compound includes a tetravalent titanium compound, preferably a soluble tetravalent titanium compound.
  • the tetravalent titanium ion formed after the tetravalent titanium compound is dissolved can be combined with a plurality of ligands to form a stable chelate compound.
  • the titanium compound includes at least one of titanium sulfate, titanium oxysulfate, titanium chloride, titanium bromide, titanium nitrate, and titanium oxychloride.
  • the gluconic acid substance includes at least one of gluconic acid, gluconate, and gluconate. Further, the gluconate includes at least one of calcium gluconate, sodium gluconate, zinc gluconate, and ferrous gluconate, and the gluconate includes gluconolactone.
  • the titanium compound may include one or both of titanyl sulfate and titanium sulfate
  • the gluconic acid may include gluconic acid, gluconolactone, calcium gluconate, sodium gluconate, zinc gluconate, gluconic acid.
  • One or more of the ferrous irons are preferably one or both of gluconic acid and gluconolactone.
  • the water-soluble new fertilizer also contains a basic substance, neutralizing the acidity of the liquid with an alkaline substance, and neutralizing until the pH of the solution is weakly acidic or neutral.
  • the above basic substance may be an organic base or an inorganic base, and the organic base includes at least one of ethanolamine, diethanolamine, triethanolamine, diethylenetriamine, triethylenetetramine, ethylenediamine, triethylamine, and isopropylamine.
  • the inorganic base includes at least one of ammonia water, potassium hydroxide, sodium hydroxide, lithium hydroxide, calcium hydroxide, magnesium hydroxide, and barium hydroxide.
  • the alkaline substance may include ammonium hydroxide, potassium hydroxide, calcium hydroxide, barium hydroxide, ethanolamine, diethanolamine, triethanolamine, diethylenetriamine, triethylenetetramine, ethylenediamine, triethylamine.
  • ammonium hydroxide potassium hydroxide
  • calcium hydroxide barium hydroxide
  • ethanolamine diethanolamine
  • triethanolamine diethylenetriamine
  • triethylenetetramine ethylenediamine
  • triethylamine triethylamine.
  • isopropylamine One or a mixture of isopropylamine.
  • the water-soluble fertilizer also includes a medium amount of elements, a combination of trace elements and water, and the mass ratio of water to titanium compound can be controlled between (4-30):1, in addition to being controlled at 5:1. , 6:1, 7:1, 8:1, 9:1, 10:1, etc.
  • the chelated trace elements include at least one of zinc, magnesium, iron, manganese, copper, cobalt, and molybdenum.
  • the present invention also provides a method for preparing the water-soluble fertilizer, which comprises: mixing gluconic acid substance with titanium compound according to a coordination molar ratio (2-5):1 to form glucose. Titanate complex.
  • the temperature at which the gluconic acid substance is mixed and coordinated with the titanium compound is 25-60 ° C, and the time is 1-3 h. Further, it further comprises: neutralizing the titanium gluconate complex with a basic substance, and sedimenting and filtering.
  • the water-soluble fertilizer preparation method of the embodiment of the invention is simple, the operation condition is mild, the mixing and the stirring are uniform, the content of each element in the obtained water-soluble fertilizer product is within the ideal index range, and there is no agglomerated small particles, because if there is agglomeration The appearance of particles is not easily absorbed by plants.
  • the gluconic acid substance is mixed with water at 25 to 60 ° C to form a mixed solution, and then the reaction is carried out to form an aqueous solution which is more advantageous for the subsequent reaction.
  • the stirring mode is high-speed shear stirring, and the stirring rate is controlled between 500-1500 rpm. .
  • the time of settling is controlled to substantially achieve the effect of sedimentation of the filtration residue between 24-48 hours.
  • the process of concentration can be concentrated by heating or concentrated by vacuum drying, and the finer the particle size control during the pulverization process, the better the subsequent addition of other elements is more conducive to the mutual compatibility of various substances.
  • the role works together.
  • the water-soluble fertilizer containing titanium gluconate complex of the present invention has high stability of a complex formed by a gluconic acid ligand and titanium ions. Under long-term normal storage conditions, no discoloration or precipitation. After freezing at -18 ° C for 1 day and storage at 50 ° C for 14 days, no hydrolysis, no precipitation, and no reduction in titanium (IV) ion content. Suitable for a wide range of applications.
  • the present invention provides a water-soluble fertilizer which firstly combines gluconic acid as a ligand to complex titanium ions to form a functional fertilizer of titanium gluconate complex, which is non-toxic and better.
  • the ground is absorbed and utilized by crops, is environmentally friendly, and the ratio of each element is more reasonable. It can improve the yield and quality of crops, and does not cause soil compaction. It has the advantages of soil control and environmental protection, and is very suitable for crop production applications;
  • the preparation method of the water-soluble fertilizer of the invention has the advantages of close connection, simple operation, no three wastes, safety and environmental protection, and the fertilizer efficiency improvement of the variety is realized by rational design of the whole preparation method, and is worthy of widespread application.
  • the specific preparation method of the water-soluble fertilizer includes the following steps:
  • the filtrate is diluted with water to a titanium ion concentration of 10.0 g / L (the determination of titanium ion concentration, according to the industry standard NYT 2879-2015 "water soluble fertilizer cobalt, titanium content determination” 5.2 titanium content determination plasma emission spectrometry specified method get on).
  • Example 2 2.0 ml of the water-soluble fertilizer of the above Example 1 was weighed as a sample, diluted with water to 1000 ml (i.e., a titanium ion concentration of 20 mg/L per sample), and then sealed and stored at room temperature to observe the time at which precipitation occurred. The sample remained clear and transparent after 7 days. After testing, the titanium ion concentration was still 20 mg/L.
  • the water-soluble fertilizer prepared in the above Example 1 was diluted with water as a sample to a titanium ion concentration of 20 mg/L, and then subjected to a field experiment.
  • the specific steps include:
  • Test crop cucumber, Jinyou 10, whose seeds were purchased from Liaoning Seed Company.
  • Test site From February to June 2016, it was carried out in the 300M2 greenhouse of Li Hongzhi, Dawangzhangzi Village, Brownpu Town, Lingyuan City, Liaoning province.
  • the test site was the local ordinary sandy bottom black soil field. Conventional water and fertilizer management.
  • Test design spraying the above samples in the three-quarter (three-zone) area of the greenhouse, planting cucumbers, spraying the first time on the 30th day after planting, and spraying the above samples to 20mg/L, the remaining four
  • the same area (contrast area) is sprayed with the same amount of water (blank control CK).
  • a second spray was applied on the 45th day after sowing, and then sprayed once every 10 days, in the same manner as above, and sprayed 5 times in total.
  • Fruit survey The top flower of cucumber fruit in the treatment area is not easy to fall off, the shape of the melon strip is straight, the diameter is enlarged by about 0.5cm, the length is increased by 3-5cm, the section of the melon heart is yellow-green, and the taste is refreshing.
  • the fruit section of the comparison area was yellowish white and the taste was poor.
  • Harvesting period survey The harvesting period is greatly extended, and the treatment area is delayed by 20-40 days than the comparison area, and more than 3-5 fruits are harvested. The yield increase can reach more than 50%.
  • the specific preparation method of the water-soluble fertilizer includes the following steps:
  • the filtrate was diluted with water to a titanium ion concentration of 10.0 g/L (the mass ratio of titanyl sulfate to water was controlled between (4-30):1). Then, the filtrate was added to a liquid EDTA cerium zinc, manganese, iron, magnesium ammonium salt solution (in which the element content is Mn + Zn + Fe + Mg ⁇ 100 g / L), and the ratio was 1:2, and the mixture was uniformly mixed.
  • the water-soluble fertilizer of the above Example 2 was diluted to a titanium ion of 10 mg/L for treating wheat. Demonstration test site: From March to May 2017, 2.1 mu of Liuyuannong block in Luying Village, Siying Township, Cheng'an County, Hebei province, and 0.7 mu of land. Wheat variety: "gas blast”. Water and fertilizer conditions: 50 kg of compound fertilizer (2-25-5). The treatment method of the treatment area is sprayed once in the jointing stage of wheat and sprayed once again in the heading stage. The fertilizer applied is: water-soluble fertilizer diluted to 10 mg/L in Example 2 and potassium dihydrogen phosphate 1 ⁇ , urea 1.5 % mixed spray. The treatment in the control zone was the same, and only the same concentration of potassium dihydrogen phosphate and urea were sprayed.
  • the specific preparation method of the water-soluble fertilizer includes the following steps:
  • the filtrate was heated and evaporated to a weight loss of about 40%, and then converted into a vacuum drying at 80 ° C, taken out as a paste, and cooled to a solid. Then, the solid is added to a mixture of solid powdered EDTA chelating zinc, manganese, iron, magnesium potassium salt and sodium octaborate (the element content of which is Mn+Zn+Fe+B+Mg ⁇ 20%), added The ratio is 1:4, and the mixture is pulverized evenly.
  • the water-soluble fertilizer prepared in the above Example 3 was diluted and dissolved in water, and diluted with water to a titanium ion of 10 mg/L and 15 mg/L for treating jujube trees.
  • the specific preparation method of the water-soluble fertilizer includes the following steps:
  • the filtrate was heated and evaporated to a weight loss of about 40%, and then converted into a vacuum drying at 80 ° C, taken out as a paste, and cooled to a solid. Then, the solid is added to a mixture of solid powdered EDTA chelating zinc, manganese, iron, magnesium potassium salt and sodium octaborate (the element content of which is Mn+Zn+Fe+B+Mg ⁇ 20%), added The ratio is 1:4, and the mixture is pulverized evenly.
  • the water-soluble fertilizer prepared in Example 4 of the present invention was also tested in the same manner as in the method of treating jujube of Example 3.
  • the water-soluble fertilizer of the invention has good fertilizer effect, is more easily absorbed by plants and crops, and has a wide range of use, and general crops, fruit trees and the like can be applied.
  • This embodiment provides a water-soluble fertilizer, and the specific preparation method comprises the following steps:
  • the filtrate is added to a liquid EDTA cerium zinc, manganese, iron, magnesium ammonium salt solution (in which the element content is Mn + Zn + Fe + Mg ⁇ 100 g / L), the ratio is 1:2, and the mixture is uniformly mixed.
  • This embodiment provides a water-soluble fertilizer, and the specific preparation method comprises the following steps:
  • titanium nitrate 200 mol was dissolved in 250 kg of water at 60 ° C, and 1000 mol of sodium gluconate was added thereto, and stirred at 60 ° C and a rotation speed of 1500 rpm for 3 hours to form a titanium gluconate complex. After aging for 1 d, 1500 mol of ammonia water was slowly added thereto, and the mixture was stirred at 60 ° C and a rotation speed of 1000 rpm for 1 hour. Settling at 60 ° C for 48 h. The precipitated insoluble matter was filtered off. The filtrate was diluted with water to a titanium ion concentration of 10.0 g/L (the mass ratio of titanium nitrate to water was controlled between (4-30):1).
  • the filtrate is added to a liquid EDTA cerium zinc, manganese, iron, magnesium, cobalt ammonium salt solution (in which the element content is Mn+Zn+Fe+Mg+Co ⁇ 100g/L), and the ratio is 1:2. ,well mixed.
  • This embodiment provides a water-soluble fertilizer, and the specific preparation method comprises the following steps:
  • the filtrate is added to the liquid EDTA ⁇ zinc, manganese, iron, magnesium, molybdenum ammonium salt solution (the element content of Mn + Zn + Fe + Mg + Mo ⁇ 100g / L), the ratio of 1:2 ,well mixed.
  • This embodiment provides a water-soluble fertilizer, and the specific preparation method comprises the following steps:
  • titanium bromide 250 mol was dissolved in 190 kg of water at 25 ° C, 700 mol of zinc gluconate was added, and the mixture was stirred at 25 ° C and 500 rpm for 1 hour to form a titanium gluconate complex. After aging for 3 days, 1000 mol of ethylenediamine was slowly added, and the mixture was stirred at 25 ° C and a rotation speed of 1000 rpm for 1 hour. Settling at 50 ° C for 24 h. The precipitated insoluble matter was filtered off. The filtrate was diluted with water to a titanium ion concentration of 10.0 g/L (the mass ratio of titanium bromide to water was controlled between (4-30):1).
  • the filtrate is added to a liquid EDTA cerium zinc, manganese, iron, magnesium ammonium salt solution (in which the element content is Mn + Zn + Fe + Mg ⁇ 100 g / L), the ratio is 1:2, and the mixture is uniformly mixed.
  • the water-soluble fertilizer prepared in Examples 5-8 was diluted and dissolved in water, and diluted with water to a titanium ion of 10 mg/L for treating jujube trees.
  • Example 5 Example 6
  • Example 7 Fruit set rate (fruit / hanging) 0.30 0.35 0.37 0.35 0.36 Yield per plant, kg 7.2 9.5 9.8 9.6 9.6 Average single fruit weight, g 8.0 9.7 10.0 9.8 10.0
  • the invention provides a water-soluble fertilizer which is non-toxic, can be better absorbed by crops, is environmentally friendly, and has a more reasonable ratio of elements, can improve the yield and quality of crops, and does not cause soil compaction. It has the advantages of soil control, green environmental protection, etc. It is very suitable for the application of crop production. At the same time, the preparation method of the water-soluble fertilizer is closely connected before and after the steps, the operation is simple, no three wastes are produced, safe and environmentally friendly, and the whole preparation method is reasonable. The design achieves the fertilizer efficiency improvement of this variety of fertilizers, and is very suitable for large-scale industrial production, which is worthy of widespread application.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Pest Control & Pesticides (AREA)
  • Soil Sciences (AREA)
  • Fertilizers (AREA)

Abstract

La présente invention concerne un engrais soluble dans l'eau et un procédé de préparation associé. L'engrais soluble dans l'eau est principalement composé d'un complexe de gluconate de titane et d'une substance alcaline, le complexe de gluconate de titane étant préparé à partir d'une substance d'acide gluconique et d'un composé de titane selon un rapport molaire de coordination de (2-5) :1. Le procédé de préparation comprend les étapes suivantes : (A) l'autorisation à la substance d'acide gluconique et au composé de titane d'être soumis à une coordination et subissent une réaction à 25-60 °C pendant 1 à 3 heures pour obtenir le complexe de gluconate de titane; (B) le vieillissement pendant 1 à 3 jours, la neutralisation, la sédimentation, le filtrage et l'ajout d'autres substances pour obtenir l'engrais soluble dans l'eau. Selon des modes de réalisation de la présente invention, de l'acide gluconique est utilisé en tant que ligand pour la première fois pour effectuer une complexation avec des ions de titane pour former un engrais fonctionnel complexe de gluconate de titane. L'engrais est non toxique, peut être mieux absorbé et utilisé par les cultures, est respectueux de l'environnement, plus raisonnable dans le dosage d'éléments et capable d'améliorer le rendement et la qualité des cultures, ne provoquerait pas le durcissement du sol, et est capable de mettre en œuvre une réhabilitation du sol et est écologique.
PCT/CN2018/076370 2017-10-20 2018-02-12 Engrais soluble dans l'eau et procédé de préparation associé WO2019075971A1 (fr)

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CN201710981097.2A CN107793262A (zh) 2017-10-20 2017-10-20 一种水溶性肥料及其制备方法

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CN107793262A (zh) * 2017-10-20 2018-03-13 日正九安科技（北京）有限公司 一种水溶性肥料及其制备方法
CN108456016A (zh) * 2018-04-13 2018-08-28 日正九安科技（北京）有限公司 一种水溶性有机钛肥及其制备方法
CN112250478B (zh) * 2020-10-29 2021-09-14 四川龙蟒福生科技有限责任公司 一种全水溶性钛肥及其制备方法

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