CN113185357A - Flower-retention and fruit-setting stable high-concentration boron fertilizer and preparation method thereof - Google Patents

Flower-retention and fruit-setting stable high-concentration boron fertilizer and preparation method thereof Download PDF

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CN113185357A
CN113185357A CN202110624995.9A CN202110624995A CN113185357A CN 113185357 A CN113185357 A CN 113185357A CN 202110624995 A CN202110624995 A CN 202110624995A CN 113185357 A CN113185357 A CN 113185357A
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parts
boric acid
weight
boron
stirring
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吴安昌
程婷婷
沈冰涛
杨双峰
周传胜
陈军
杨明明
张卫卫
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Anhui Huilong Group Wuhe Ecological Fertilizer Industry Co ltd
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Anhui Huilong Group Wuhe Ecological Fertilizer Industry Co ltd
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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
    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
    • C05D9/00—Other inorganic fertilisers
    • C05D9/02—Other inorganic fertilisers containing trace elements
    • 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

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  • Inorganic Chemistry (AREA)
  • Fertilizers (AREA)

Abstract

A stable flower-protecting and fruit-setting high-concentration boric fertilizer comprises, by weight, 43-74 parts of boric acid, 26-57 parts of a ligand solvent and 0.01 part of a defoaming agent; the ligand solvent comprises the following components in parts by weight: 4-44 parts of water, 0.01-1 part of copper sulfate pentahydrate, 0.01-1 part of modified potassium fulvate and 12-20 parts of N, N-dimethyl-1,3-propane diamine. The preparation method comprises the following steps: dissolving copper sulfate pentahydrate in water completely, adding modified potassium fulvate, stirring at normal temperature for 15min, adding N, N-dimethyl-1,3-propane diamine into the solution, and stirring for 30min to obtain ligand solvent; and adding boric acid into the obtained ligand solvent while stirring, stirring for 1-2 h for completely dissolving the boric acid, then adding a defoaming agent, and continuously stirring for 15min to obtain a solution, namely the flower-retaining and fruit-setting stable high-concentration boron fertilizer. The fertilizer has the effects of flower retention and fruit setting and is good in stability. And the preparation method is simple and easy to operate.

Description

Flower-retention and fruit-setting stable high-concentration boron fertilizer and preparation method thereof
Technical Field
The invention relates to a stable high-concentration boron fertilizer with flower protection and fruit setting functions and a preparation method thereof.
Background
Boron is a necessary trace nutrient element for crops, has specific physiological functions and functions in the growth process of the crops, cannot be replaced by other nutrient elements, and can strengthen certain important physiological functions of the crops although not being a composition component of various organic matters in the crops. Sufficient boron supply, luxuriant plant growth, full seeds, good root system and high yield; on the contrary, the supply of boron is insufficient, the plant growth is poor, and the quality and the yield of the product are reduced; when the boron is seriously deficient, even the particles are not harvested. Especially has obvious yield increasing effect and quality improvement on boron deficiency sensitive crops, such as rape, cotton, peanut, soybean, sunflower, beet, vegetables, fruit trees and the like.
At present, the boron fertilizer is relatively complete in variety and comprises particles, powder and liquid. The particle is mainly used for basal application, the powder can be used for foliage spraying, but the solubility is small, and the liquid boron fertilizer has high intersolubility with water and can be quickly absorbed by plant leaves, so that the utilization rate of the boron fertilizer is greatly improved. Although the boron content of the existing liquid boron fertilizer in the market can reach 150g/L, the specific gravity is about 1.35, and the boron accounts for about 11 percent (by weight), the storage stability is insufficient, particularly, the crystallization is generated in a low-temperature environment, certain difficulty is met in actual popularization, and the liquid boron fertilizer cannot be widely applied and popularized.
For example, chinese patent application No. 200610022116.0, entitled method for preparing liquid boron fertilizer with surface activity, discloses that liquid boron fertilizer is prepared by mixing at least one of borax, boric acid, and boron trioxide with an organic complex and water, heating and refluxing, although liquid boron fertilizer with higher boron content is obtained, the preparation process is complicated, heating and refluxing are required, and the scheme is used to prepare liquid boron fertilizer with higher boron content and has poor storage stability; the Chinese patent application No. 201010251569.7, named as a liquid boron fertilizer and a preparation method thereof, discloses that the liquid boron fertilizer is obtained by mixing ethanolamine with water and then adding boric acid and stirring, although the production process of the boron fertilizer can be optimized and the boron weight percentage is increased by 10-12% by the technical scheme, when the boron content needs to be prepared to be higher, the boron content is particularly over 11% or 150g/L, the solution is easy to crystallize, particularly in a low-temperature environment, a spray head is easy to block in the actual application process, and the wide application and popularization are not facilitated.
Disclosure of Invention
The invention aims to solve the first technical problem of providing a stable high-concentration boron fertilizer for flower retention and fruit setting, which has the flower retention and fruit setting effects and better stability.
The second technical problem to be solved by the invention is to provide a preparation method of the flower-protecting and fruit-setting stable high-concentration boron fertilizer, which is simple and easy to operate.
In order to solve the first technical problem, the invention provides a stable flower-keeping and fruit-setting high-concentration boron fertilizer which comprises 43-74 parts by weight of boric acid, 26-57 parts by weight of a ligand solvent and 0.01 part by weight of a defoaming agent;
the ligand solvent comprises the following components in parts by weight: 4-44 parts of water, 0.01-1 part of copper sulfate pentahydrate, 0.01-1 part of modified potassium fulvate and 12-20 parts of N, N-dimethyl-1,3-propane diamine.
Preferably, the anti-foaming agent comprises 43-69 parts by weight of boric acid, 31-57 parts by weight of ligand solvent and 0.01 part by weight of defoaming agent;
the ligand solvent comprises the following components in parts by weight: 10.9-44 parts of water, 0.01-0.8 part of copper sulfate pentahydrate, 0.01-0.8 part of modified potassium fulvate and 12-18.5 parts of N, N-dimethyl-1,3-propane diamine.
Preferably, the anti-foaming agent comprises 43-63 parts by weight of boric acid, 37-57 parts by weight of ligand solvent and 0.01 part by weight of defoaming agent;
the ligand solvent comprises the following components in parts by weight: 18.4-44 parts of water, 0.01-0.8 part of copper sulfate pentahydrate, 0.01-0.8 part of modified potassium fulvate and 12-17 parts of N, N-dimethyl-1,3-propane diamine.
Preferably, the anti-foaming agent comprises 43-52 parts of boric acid, 48-57 parts of ligand solvent and 0.01 part of defoaming agent by weight;
the ligand solvent comprises the following components in parts by weight: 32.6-44 parts of water, 0.01-0.7 part of copper sulfate pentahydrate, 0.01-0.7 part of modified potassium fulvate and 12-17 parts of N, N-dimethyl-1,3-propane diamine.
The N, N-dimethyl-1,3-propane diamine is purchased from https:// chemicals. thermofisher. cn/, English name N, N-dimethyl-1,3-propane diamine, molecular formula: c5H14N2Molecular weight 102, purity 99%, CAS: 109-55-7.
The defoaming agent is polyoxypropylene glycerol ether, bubbles generated in the stirring process of the high-concentration boron fertilizer are eliminated, and the high-concentration boron fertilizer is convenient to subpackage and store.
For the sake of simple explanation, the stable high-concentration boron fertilizer with flower retention and fruit setting of the present invention is simply referred to as "boron fertilizer".
The boron fertilizer has the advantages that: the boron fertilizer has high concentration and strong stability, and not only provides boron element, but also provides copper, potassium fulvate and other nutrient components.
In order to solve the second technical problem, the invention provides a preparation method of the flower-keeping and fruit-setting stable high-concentration boron fertilizer, which comprises the following steps:
(1) dissolving copper sulfate pentahydrate in water completely according to a certain proportion, adding modified potassium fulvate, stirring at normal temperature for 15min, adding N, N-dimethyl-1,3-propane diamine into the solution, and continuously stirring for 30min to obtain a ligand solvent;
(2) and (2) adding boric acid into the ligand solvent obtained in the step (1) while stirring, stirring for 1-2 h for complete dissolution of the boric acid, then adding a defoaming agent, and continuously stirring for 15min to obtain a uniform solution, namely the stable high-concentration boron fertilizer for flower retention and fruit setting.
For the sake of simple explanation, the preparation method of the flower-keeping and fruit-setting stable high-concentration boron fertilizer of the present invention is simply referred to as the present method below.
The method has the advantages that: the method has simple production process, can be used for production at normal temperature, and has low equipment requirement.
Detailed Description
Example 1
The stable high-concentration boron fertilizer comprises 43g of boric acid, 44g of water, 0.5g of copper sulfate pentahydrate, 0.5g of modified potassium fulvate, 12g of N, N-dimethyl-1,3-propane diamine and 0.01g of defoaming agent in parts by weight;
the preparation method comprises the following steps:
(1) dissolving 0.5g of blue vitriod in 44g of water completely according to the proportion, adding 0.5g of modified potassium fulvate, stirring for 15min at normal temperature, adding 12g N, N-dimethyl-1,3-propane diamine into the solution, and continuously stirring for 30min to obtain a ligand solvent;
(2) adding 43g of boric acid into the ligand solvent obtained in the step (1) in batches while stirring, stirring for 1h for completely dissolving the boric acid, then adding 0.01g of defoaming agent, and continuously stirring for 15min to obtain a solution, namely a stable high-concentration boron fertilizer with flower and fruit retention property, which is marked as boron fertilizer I;
through detection, the boric acid in the boron fertilizer I accounts for 43% by mass, the boron accounts for 7.5% by mass, and the boron concentration is 100 g/L;
example 2
The stable high-concentration boron fertilizer comprises, by weight, 49g of boric acid, 37g of water, 0.5g of copper sulfate pentahydrate, 0.5g of modified potassium fulvate, 13g of N, N-dimethyl-1,3-propane diamine and 0.01g of defoaming agent;
the preparation method comprises the following steps:
(1) dissolving 0.5g of blue vitriod in 37g of water completely according to the proportion, adding 0.5g of modified potassium fulvate, stirring for 15min at normal temperature, adding 13g N, N-dimethyl-1,3-propane diamine into the solution, and continuously stirring for 30min to obtain a ligand solvent;
(2) adding 49g of boric acid into the ligand solvent in the step (1) in batches while stirring, stirring for 1h for complete dissolution of the boric acid, then adding 0.01g of defoaming agent, and continuously stirring for 15min to obtain a solution, namely a stable high-concentration boron fertilizer with flower retention and fruit setting, which is marked as boron fertilizer II;
according to detection, in the boron fertilizer II, the mass percent of boric acid is 49%, the mass percent of boron is 8.5%, and the mass concentration of boron is 110 g/L;
example 3
The stable high-concentration boron fertilizer comprises, by weight, 52g of boric acid, 32.6g of water, 0.7g of copper sulfate pentahydrate, 0.7g of modified potassium fulvate, 14g of N, N-dimethyl-1,3-propane diamine and 0.01g of a defoaming agent;
the preparation method comprises the following steps:
(1) dissolving 0.7g of blue vitriod in 32.6g of water completely according to the proportion, adding 0.7g of modified potassium fulvate, stirring for 15min at normal temperature, adding 14g N, N-dimethyl-1,3-propane diamine into the solution, and continuously stirring for 30min to obtain a ligand solvent;
(2) adding 52g of boric acid into the ligand solvent in the step (1) in batches while stirring, stirring for 1.5h for complete dissolution of the boric acid, then adding 0.01g of defoaming agent, and continuously stirring for 15min to obtain a solution, namely a stable high-concentration boron fertilizer with flower retention and fruit setting, which is marked as boron fertilizer III;
according to detection, in the boron fertilizer III, the mass percent of boric acid is 52%, the mass percent of boron is 9%, and the mass concentration of boron is 120 g/L;
example 4
The stable high-concentration boron fertilizer comprises, by weight, 58g of boric acid, 25.1g of water, 0.7g of copper sulfate pentahydrate, 0.7g of modified potassium fulvate, 15.5g of N, N-dimethyl-1,3-propane diamine and 0.01g of a defoaming agent;
the preparation method comprises the following steps:
(1) dissolving 0.7g of blue vitriod in 25.1g of water completely according to the proportion, adding 0.7g of modified potassium fulvate, stirring for 15min at normal temperature, adding 15.5g N, N-dimethyl-1,3-propane diamine into the solution, and continuously stirring for 30min to obtain a ligand solvent;
(2) adding 58g of boric acid into the ligand solvent in the step (1) in batches while stirring, stirring for 1.5h for complete dissolution of the boric acid, then adding 0.01g of defoaming agent, and continuously stirring for 15min to obtain a solution, namely a stable high-concentration boron fertilizer with flower protection and fruit setting, which is marked as boron fertilizer IV;
according to detection, the boric acid in the boric fertilizer IV accounts for 58% by mass, the boron accounts for 10% by mass, and the boron concentration is 135 g/L;
example 5
The stable high-concentration boron fertilizer comprises, by weight, 63g of boric acid, 18.4g of water, 0.8g of copper sulfate pentahydrate, 0.8g of modified potassium fulvate, 17g of N, N-dimethyl-1,3-propane diamine and 0.01g of defoaming agent;
the preparation method comprises the following steps:
(1) dissolving 0.8g of blue vitriod in 18.4g of water completely according to the proportion, adding 0.8g of modified potassium fulvate, stirring for 15min at normal temperature, adding 17g N, N-dimethyl-1,3-propane diamine into the solution, and continuously stirring for 30min to obtain a ligand solvent;
(2) adding 63g of boric acid into the ligand solvent in the step (1) in batches while stirring, stirring for 1.5h for complete dissolution of the boric acid, then adding 0.01g of defoaming agent, and continuously stirring for 15min to obtain a solution, namely a stable high-concentration boron fertilizer with flower protection and fruit setting, which is marked as boron fertilizer V;
according to detection, in the boron fertilizer V, the mass percent of boric acid is 63%, the mass percent of boron is 11%, and the mass concentration of boron is 150 g/L;
example 6
The stable high-concentration boron fertilizer comprises 69g of boric acid, 10.9g of water, 0.8g of copper sulfate pentahydrate, 0.8g of modified potassium fulvate, 18.5g of N, N-dimethyl-1,3-propane diamine and 0.01g of defoaming agent in parts by weight;
the preparation method comprises the following steps:
(1) dissolving 0.8g of blue vitriod in 10.9g of water completely according to the proportion, adding 0.8g of modified potassium fulvate, stirring for 15min at normal temperature, adding 18.5g N, N-dimethyl-1,3-propane diamine into the solution, and continuously stirring for 30min to obtain a ligand solvent;
(2) adding 69g of boric acid into the ligand solvent in the step (1) in batches while stirring, stirring for 2 hours until the boric acid is completely dissolved, then adding 0.01g of defoaming agent, and continuously stirring for 15 minutes to obtain a solution, namely a stable high-concentration boron fertilizer with flower and fruit retention property, which is marked as a boron fertilizer VI;
according to detection, in the boron fertilizer VI, the mass percent of boric acid is 69%, the mass percent of boron is 12%, and the mass concentration of boron is 165 g/L;
example 7
The stable high-concentration boron fertilizer comprises 74g of boric acid, 4g of water, 1g of copper sulfate pentahydrate, 1g of modified potassium fulvate, 20g of N, N-dimethyl-1,3-propane diamine and 0.01g of defoaming agent in parts by weight;
the preparation method comprises the following steps:
(1) 1g of blue vitriol is completely dissolved in 4g of water according to the proportion, 1g of modified potassium fulvate is added, stirring is carried out for 15min at normal temperature, 20g N, N-dimethyl-1,3-propane diamine is added into the solution, and stirring is carried out for 30min to obtain a ligand solvent;
(2) adding 74g of boric acid into the ligand solvent in the step (1) in batches while stirring, stirring for 2h for completely dissolving the boric acid, then adding 0.01g of defoaming agent, and continuously stirring for 15min to obtain a solution, namely a stable high-concentration boron fertilizer with flower retention and fruit setting, which is marked as boron fertilizer VII;
according to detection, the boric acid in the boron fertilizer VII accounts for 74% by mass, the boron accounts for 13% by mass, and the boron concentration accounts for 180 g/L;
the invention is characterized in that the modified potassium fulvate is obtained by a method for preparing modified humate in an invention patent granted under the application number ZL 201711106506.0.
Through detection, the stable flower-retaining fruit-setting high-concentration boron fertilizers I to VII, B of which is more than or equal to 100g/L, conform to microelement water-soluble fertilizer NY/T1428-:
table 1 examples used raw material ratios and boron contents of boron fertilizers
Figure BDA0003101841150000071
Comparative storage experiment:
1) sample (I)
A commercially available 150g/L boron fertilizer sample, the boron fertilizers I to VII provided in the above examples 1 to 8, and the boron fertilizers I-1, I-2, II-1, II-2, III-1, V-1, VI-1 and VII-1 provided in the comparative examples 1 to 8, wherein the preparation process of the boron fertilizers in the comparative examples is as follows:
comparative example 1
The boric fertilizer comprises 43g of boric acid, 57g of water and 0.01g of defoaming agent;
the preparation process of the boric fertilizer comprises the following steps:
adding 43g of boric acid into water in batches while stirring according to a proportion, gradually generating crystals at the bottom of the solution along with stirring, slowing down the dissolving speed of the boric acid until the boric acid is insoluble, and obtaining a mixed system of the solution and the boric acid crystals, namely the boric fertilizer I-1;
in the boric fertilizer I-1, the mass percent of boric acid is 43 percent, and the mass percent of boron is 7.5 percent.
Comparative example 2
The boric fertilizer comprises 43g of boric acid, 45g of water, 12g of N, N-dimethyl-1,3-propane diamine and 0.01g of defoaming agent;
the preparation process of the boric fertilizer comprises the following steps:
step 1: stirring and adding 12g N, N-dimethyl-1,3-propane diamine into 45g of water according to the proportion, and continuously stirring for 30min to obtain a ligand solvent;
step 2: then adding 43g of boric acid into the ligand solvent in the step 1 in batches while stirring, slowly dissolving the boric acid with stirring until the boric acid is completely dissolved, then adding 0.01g of defoaming agent, and continuously stirring for 15min to obtain a boron fertilizer I-2;
in the boric fertilizer I-2, the mass percent of boric acid is 43%, the mass percent of boron is 7.5%, and the mass concentration of boron is 100 g/L.
Comparative example 3
The boric fertilizer comprises 49g of boric acid, 38g of water, 13g of N, N-dimethyl-1,3-propane diamine and 0.01g of defoaming agent;
the preparation process of the boric fertilizer comprises the following steps:
step 1: adding 13g N, N-dimethyl-1,3-propane diamine into 38g of water in proportion by stirring, and continuously stirring for 30min to obtain a ligand solvent;
step 2: then adding 49g of boric acid into the ligand solvent in the step 1 in batches while stirring, completely dissolving the boric acid within 1.5h with stirring, adding 0.01g of defoaming agent, and continuously stirring for 15min to obtain a boron fertilizer II-1;
in the boron fertilizer II-1, the mass percent of boric acid is 49%, the mass percent of boron is 8.5%, and the mass concentration of boron is 110 g/L.
Comparative example 4
The boric fertilizer comprises 49g of boric acid, 37.5g of water, 0.5g of copper sulfate pentahydrate, 13g of N, N-dimethyl-1,3-propane diamine and 0.01g of defoaming agent;
the preparation process of the boric fertilizer comprises the following steps:
step 1: dissolving 0.5g of blue vitriol in 37.5g of water completely according to the proportion, stirring for 15min at normal temperature, adding 13g N, N-dimethyl-1,3-propane diamine into the solution, and continuously stirring for 30min to obtain a ligand solvent;
step 2: then adding 49g of boric acid into the ligand solvent in the step (1) in batches while stirring, completely dissolving the boric acid within 1.5h with stirring, adding 0.01g of defoaming agent, and continuously stirring for 15min to obtain a boron fertilizer II-2;
in the boron fertilizer II-2, the mass percent of boric acid is 49%, the mass percent of boron is 8.5%, and the mass concentration of boron is 110 g/L.
Comparative example 5
The boric fertilizer comprises 52g of boric acid, 33.3g of water, 0.7g of copper sulfate pentahydrate, 14g of N, N-dimethyl-1,3-propane diamine and 0.01g of defoaming agent;
the preparation process of the boric fertilizer comprises the following steps:
step 1: dissolving 0.7g of blue vitriol in 33.3g of water completely according to the proportion, stirring for 15min at normal temperature, adding 14g N, N-dimethyl-1,3-propane diamine into the solution, and continuously stirring for 30min to obtain a ligand solvent;
step 2: then adding 52g of boric acid into the ligand solvent in the step 1 in batches while stirring, completely dissolving the boric acid within 2h with stirring, then adding 0.01g of defoaming agent, and continuously stirring for 15min to obtain a boric fertilizer III-1;
the boric acid in the boric fertilizer accounts for 52% by mass, the boron accounts for 9% by mass, and the boron concentration is 120 g/L.
Comparative example 6
The boric fertilizer comprises 63g of boric acid, 19.2g of water, 0.8g of copper sulfate pentahydrate, 17g of N, N-dimethyl-1,3-propane diamine and 0.01g of defoaming agent;
the preparation process of the boric fertilizer comprises the following steps:
step 1: dissolving 0.8g of blue vitriol in 19.2g of water completely according to the proportion, stirring for 15min at normal temperature, adding 17g N, N-dimethyl-1,3-propane diamine into the solution, and continuously stirring for 30min to obtain a ligand solvent;
step 2: then adding 63g of boric acid into the ligand solvent in the step 1 in batches while stirring, completely dissolving the boric acid within 3 hours with stirring, adding 0.01g of defoaming agent, and continuously stirring for 15min to obtain a boron fertilizer V-1;
the boric acid in the boron fertilizer accounts for 63% by mass, the boron accounts for 11% by mass, and the boron concentration is 150 g/L.
Comparative example 7
The boric fertilizer comprises 69g of boric acid, 11.7g of water, 0.8g of copper sulfate pentahydrate, 18.5g of N, N-dimethyl-1,3-propane diamine and 0.01g of defoaming agent;
the preparation process of the boric fertilizer comprises the following steps:
step 1: dissolving 0.8g of blue vitriol in 11.7g of water completely according to the proportion, stirring for 15min at normal temperature, adding 18.5g N, N-dimethyl-1,3-propane diamine into the solution, and continuously stirring for 30min to obtain a ligand solvent;
step 2: then adding 69g of boric acid into the ligand solvent in the step 1 in batches while stirring, and slowing the dissolving speed of the boric acid along with stirring until the boric acid is insoluble to obtain a boric acid solvent mixed opaque system with higher viscosity, so as to obtain a boric fertilizer VI-1;
the boric acid in the boron fertilizer accounts for 69% by mass, and the boron accounts for 12% by mass.
Comparative example 8
The boric fertilizer comprises 74g of boric acid, 5g of water, 1g of copper sulfate pentahydrate, 20g of N, N-dimethyl-1,3-propane diamine and 0.01g of defoaming agent;
the preparation process of the boric fertilizer comprises the following steps:
step 1: dissolving 1g of blue vitriol completely in 5g of water according to a proportion, stirring for 15min at normal temperature, adding 20g N, N-dimethyl-1,3-propane diamine into the solution, and continuously stirring for 30min to obtain a ligand solvent;
step 2: then adding 74g of boric acid into the ligand solvent in the step 1 in batches while stirring, and slowing the dissolving speed of the boric acid along with stirring until the boric acid is insoluble to obtain a boric acid solvent mixed opaque system with high viscosity, so as to obtain a boron fertilizer VII-1;
the boric acid in the boron fertilizer accounts for 74% by mass, and the boron accounts for 13% by mass.
The specific addition amounts and contents of the boron fertilizers in the comparative examples 1-8 are shown in the following table 2:
TABLE 2 comparison of raw material ratios and boron contents used in boron fertilizers
Figure BDA0003101841150000111
2) Device
A constant temperature box, DGF-9050A type, Yangzhou Hui Ke electronics Limited company;
BCD-228D11SY, Haixin Sound (Guangdong) refrigerator, Inc.;
3) experimental methods
The boron fertilizer participating in the experiment is subjected to a storage experiment, stored for 2 months at-7, 4, 25 and 54 ℃, whether the bottom of the solution is crystallized or precipitated is observed, the stability of the experimental sample is examined, and the storage result is shown in the following table 3.
TABLE 3 storage of different boron fertilizer samples
Figure BDA0003101841150000121
Note: "none" means no crystallization or precipitation was found during the storage experiment;
b. a few50"means that a small amount of crystals or precipitates are found out on the 50 th day during the storage experiment, and a large amount of crystals or precipitates are generated after the storage is continued after the small amount of crystals or precipitates appear;
c. "having0"means that the sample is not completely dissolved or that a large amount of crystals, precipitates, has been generated before storage.
From the storage experiments, it can be seen from table 3:
1. no crystallization or precipitation is found in the whole storage process of the boron fertilizers I-V, which shows that the boron fertilizers I-V provided by the invention have better stability, the mass percent of boric acid is 43-63%, the mass percent of boron is 7.5-11%, the mass concentration of boron is 100-150 g/L, the boron fertilizers all meet the technical index requirements of the agricultural standard NY/T1428-;
2. in the whole process of storage, a small amount of crystals or precipitates are found in 50 days and 30 days when the boron fertilizers VI and VII are stored at minus 7 ℃, a small amount of crystals or precipitates are found in 50 days when the boron fertilizers VII are stored at 4 ℃, and a small amount of crystals or precipitates are not found at other temperatures, so that the boron fertilizers VI and VII provided by the invention have certain stability, a small amount of crystals can be generated at low temperature, the mass percentages of boric acid are 69% and 74%, the mass percentages of boron are 12% and 13%, the mass concentrations of boron are 165g/L and 180g/L, and the boron fertilizers VI and VII can be applied in seasons with higher temperature or areas with higher temperature;
3. according to the boron fertilizer I-1 provided by the comparative example 1, as the solubility of boric acid at normal temperature is 5.6g/100mL, the addition amount of the boric acid in the comparative example 1 is far more than the solubility, the boric acid can not be completely dissolved under the condition that no other solvent is added except water, or the content of boron in a dissolved boric acid solution is low, so that the technical index requirements of the agricultural standard NY/T1428-;
4. according to the boron fertilizers I-2 and II-1 provided by the comparative examples 2 and 3, N-dimethyl-1,3-propane diamine is added into water as a ligand solvent, the boric acid and the N, N-dimethyl-1,3-propane diamine remarkably improve the solubility of the boric acid under the action of Van der Waals force (hydrogen bond or coordinate bond), the mass percentages of the boric acid after complete dissolution are respectively 43% and 49%, the mass percentages of boron are respectively 7.5% and 8.5%, the mass concentrations of boron are respectively 100g/L and 110g/L, the boron fertilizer II-1 is stored at-7 ℃ and 4 ℃ for 30 days and 45 days respectively to find a small amount of crystallization or precipitation, and no small amount of crystallization or precipitation is found at other temperatures, which indicates that the boron fertilizers I-2 and II-1 provided by the comparative examples 2 and 3 have certain stability when the boron content is low, but when the concentration of the boron fertilizer is increased, the stability is deteriorated;
5. according to the boron fertilizer II-2 provided by the comparative example 4, N-dimethyl-1,3-propane diamine and blue vitriol are added into water as ligand solvent, boric acid and N, N-dimethyl-1,3-propane diamine have empty orbits capable of accommodating electron pairs outside a copper ion nucleus under the action of Van der Waals force (hydrogen bonds or coordination bonds), boric acid and N, N-dimethyl-1,3-propane diamine can provide lone electron pairs to enter the empty orbits for complex reaction, a stable structure is formed, the solubility of boric acid is improved, the mass percentage of boric acid after complete dissolution is 49%, the mass percentage of boron is 8.5%, the mass concentration of boron is 110g/L, no crystallization is found at normal temperature, 54 ℃ and 4 ℃, a small amount of crystallization or precipitation is found at 50 days after-7 ℃ storage, the storage stability of the boron fertilizer II-2 provided by the comparative example 4 is improved to a certain extent after copper ions are added into a ligand solvent compared with the boron fertilizer II-2 provided by the comparative example 3;
6. according to the boron fertilizers III-1 to VII-1 provided by the comparative examples 5 to 8, copper ions are added into ligand solvents, but the storage stability is gradually weakened along with the increase of boron concentration, and the storage days for a small amount of crystallization or precipitation are found to be less when the concentration is higher, which indicates that the copper ions can enhance the stability of a boron fertilizer system to a certain extent, but the stability is poor when the boron fertilizer concentration is increased, particularly when the mass concentration exceeds 150g/L, and the production and subpackaging can hardly be carried out;
7. however, in the boron fertilizers I-V provided by the invention, in addition to adding N, N-dimethyl-1,3-propane diamine and copper sulfate pentahydrate and modified potassium fulvate in a ligand solvent, the modified potassium fulvate is modified by oxidation, the active functional group is increased, the active functional group of an electron pair and the active functional group of an electron-withdrawing pair are increased, the van der Waals force between the groups can be further increased in a solution, the solubility of boric acid is increased, the stability of a system is improved, and no crystallization or precipitation phenomenon is found in a storage experiment for 2 months;
8. in the whole storage process, a small amount of crystals or precipitates are found in the boron fertilizers VI and VII which are stored for 50 days and 30 days at-7 ℃, a small amount of crystals or precipitates are found in the boron fertilizer VII which is stored for 50 days at 4 ℃, and a small amount of crystals or precipitates are not found at other temperatures, which indicates that when the boron concentration continues to rise, the stability of the boron fertilizer is gradually weakened, a ligand solvent has a dissolution interval for boric acid, and the stability is weakened when the dissolution interval exceeds the highest limit;
9. according to the storage condition of the boron fertilizer purchased in the market, no crystallization or precipitation phenomenon is found under the conditions of normal temperature and 54 ℃, but when the temperature is reduced to 4 ℃ and-7 ℃, the crystallization or precipitation phenomenon is found in 14 th and 7 th days of storage, which indicates that the boron fertilizer purchased in the market has unstable properties, and particularly, when the temperature is low, the crystallization occurs, but the boron fertilizer with the same concentration as the boron fertilizer provided by the invention has no crystallization or precipitation phenomenon in the storage process, so that the boron fertilizer provided by the invention has strong stability.
In conclusion, the solubility of boric acid in water is low, in order to increase the solubility, a ligand solvent is prepared in advance, the ligand solvent comprises water, copper ions, modified potassium fulvate and N, N-dimethyl-1,3-propanediamine, the boric acid and the ligand solvent are mutually cooperated, and the borate generated between the boric acid and the ligand is enhanced through the van der Waals force (hydrogen bond or coordinate bond) effect to improve the system stability, the boron content provided by the application is 100 g/L-150 g/L and is a stable system, the boron content is 165 g/L-180 g/L and is a common stable system, and the boron-containing boron-modified potassium fulvate is suitable for being applied in areas with slightly high temperature or seasons.
While there have been shown and described the fundamental principles of the invention, the principal features thereof, and the advantages thereof, it will be understood by those skilled in the art that the invention is not limited by the embodiments described above, which are given by way of illustration of the principles of the invention, but is capable of numerous changes and modifications without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (5)

1. The flower-protecting and fruit-setting stable high-concentration boron fertilizer is characterized in that: the composite material comprises 43-74 parts by weight of boric acid, 26-57 parts by weight of ligand solvent and 0.01 part by weight of defoaming agent;
the ligand solvent comprises the following components in parts by weight: 4-44 parts of water, 0.01-1 part of copper sulfate pentahydrate, 0.01-1 part of modified potassium fulvate and 12-20 parts of N, N-dimethyl-1,3-propane diamine.
2. The stable high-concentration boron fertilizer with flower protection and fruit setting functions as claimed in claim 1, wherein: the composite material comprises 43-69 parts by weight of boric acid, 31-57 parts by weight of ligand solvent and 0.01 part by weight of defoaming agent;
the ligand solvent comprises the following components in parts by weight: 10.9-44 parts of water, 0.01-0.8 part of copper sulfate pentahydrate, 0.01-0.8 part of modified potassium fulvate and 12-18.5 parts of N, N-dimethyl-1,3-propane diamine.
3. The stable high-concentration boron fertilizer with flower protection and fruit setting functions as claimed in claim 2, wherein: the anti-foaming agent comprises 43-63 parts by weight of boric acid, 37-57 parts by weight of ligand solvent and 0.01 part by weight of defoaming agent;
the ligand solvent comprises the following components in parts by weight: 18.4-44 parts of water, 0.01-0.8 part of copper sulfate pentahydrate, 0.01-0.8 part of modified potassium fulvate and 12-17 parts of N, N-dimethyl-1,3-propane diamine.
4. The stable high-concentration boron fertilizer with flower protection and fruit setting functions as claimed in claim 3, wherein: the composite material comprises 43-52 parts by weight of boric acid, 48-57 parts by weight of ligand solvent and 0.01 part by weight of defoaming agent;
the ligand solvent comprises the following components in parts by weight: 32.6-44 parts of water, 0.01-0.7 part of copper sulfate pentahydrate, 0.01-0.7 part of modified potassium fulvate and 12-17 parts of N, N-dimethyl-1,3-propane diamine.
5. The method for preparing the flower-protecting and fruit-setting stable high-concentration boron fertilizer according to any one of claims 1 to 4, characterized by comprising the following steps:
(1) dissolving copper sulfate pentahydrate in water completely according to a certain proportion, adding modified potassium fulvate, stirring at normal temperature for 15min, adding N, N-dimethyl-1,3-propane diamine into the solution, and continuously stirring for 30min to obtain a ligand solvent;
(2) and (2) adding boric acid into the ligand solvent obtained in the step (1) while stirring, stirring for 1-2 h for complete dissolution of the boric acid, then adding a defoaming agent, and continuously stirring for 15min to obtain a uniform solution, namely the stable high-concentration boron fertilizer for flower retention and fruit setting.
CN202110624995.9A 2021-06-04 2021-06-04 Flower-retention and fruit-setting stable high-concentration boron fertilizer and preparation method thereof Pending CN113185357A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1903801A (en) * 2006-07-31 2007-01-31 朱建烨 Method of preparing liquid boron fertilizer
CN102432383A (en) * 2011-09-22 2012-05-02 陕西鼎天济农腐殖酸制品有限公司 Humic acid organic boron fertilizer and production method thereof
CN102584410A (en) * 2011-01-07 2012-07-18 徐巍 Novel preparation method of liquid boron fertilizer and liquid boron fertilizer
CN102850112A (en) * 2012-08-01 2013-01-02 乌鲁木齐中汇国豪生物科技有限公司 Method for preparing liquid boric fertilizer
CN107298608A (en) * 2017-06-27 2017-10-27 刘磊 A kind of preparation method of liquid boron fertilizer

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1903801A (en) * 2006-07-31 2007-01-31 朱建烨 Method of preparing liquid boron fertilizer
CN102584410A (en) * 2011-01-07 2012-07-18 徐巍 Novel preparation method of liquid boron fertilizer and liquid boron fertilizer
CN102432383A (en) * 2011-09-22 2012-05-02 陕西鼎天济农腐殖酸制品有限公司 Humic acid organic boron fertilizer and production method thereof
CN102850112A (en) * 2012-08-01 2013-01-02 乌鲁木齐中汇国豪生物科技有限公司 Method for preparing liquid boric fertilizer
CN107298608A (en) * 2017-06-27 2017-10-27 刘磊 A kind of preparation method of liquid boron fertilizer

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