CN113582770A - Slow-release long-acting compound fertilizer for corn planting and preparation method thereof - Google Patents
Slow-release long-acting compound fertilizer for corn planting and preparation method thereof Download PDFInfo
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- CN113582770A CN113582770A CN202110926691.8A CN202110926691A CN113582770A CN 113582770 A CN113582770 A CN 113582770A CN 202110926691 A CN202110926691 A CN 202110926691A CN 113582770 A CN113582770 A CN 113582770A
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C11/00—Other nitrogenous fertilisers
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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
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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
- C05G3/80—Soil conditioners
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
- C05G3/90—Mixtures of one or more fertilisers with additives not having a specially fertilising activity for affecting the nitrification of ammonium compounds or urea in the soil
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- 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
- C05G5/14—Tablets, spikes, rods, blocks or balls
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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
- 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
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Abstract
The invention discloses a slow-release long-acting compound fertilizer for corn planting and a preparation method thereof, wherein the slow-release long-acting compound fertilizer comprises a coating and a built-in fertilizer, and the coating comprises the following components in parts by weight: 30-42 parts of slow release resin, 20-36 parts of water-absorbent resin, 12-18 parts of inorganic salt and 1-5 parts of pullulan. According to the invention, through the structural arrangement of the built-in fertilizer, the slow release resin and the water absorbent resin from inside to outside and the inorganic salt contained in the built-in fertilizer, when the prepared compound fertilizer is used, the water absorbent resin slowly releases the inorganic salt in the first stage, the water absorbent resin is degraded in the second stage to expose the slow release resin, the slow release resin starts to degrade and release the inorganic salt, the slow release resin in the third stage is degraded to form pores, and the built-in fertilizer flows out, so that the controlled release of nutrients by the compound fertilizer is realized, wherein the inorganic salt components in the water absorbent resin, the slow release resin and the built-in fertilizer can be subjected to different component arrangement according to the growth requirements of plants, so that the nutrient requirements of the plants in different growth stages are met, and the lasting and comprehensive nutrients are provided.
Description
Technical Field
The invention relates to the technical field of slow release fertilizers, in particular to a slow release long-acting compound fertilizer for corn planting and a preparation method thereof.
Background
Corn is an important grain crop, is an important feed source for animal husbandry, aquaculture and the like, and is one of indispensable raw materials for food, medical treatment and health, light industry, chemical industry and the like; there is a large demand for nutrients throughout its growth cycle. The fertilizer can provide nutrient elements necessary for plants for corn, can improve soil property and soil fertility level, is a material foundation for agricultural production and garden cultivation, comprises ammonium phosphate fertilizer, macroelement water-soluble fertilizer, secondary element fertilizer, biological fertilizer, organic fertilizer, multi-dimensional field energy concentrated organic fertilizer and the like, and can be classified into water-soluble fertilizer, slow-release fertilizer and the like. Wherein the fertilizer is slowly released. The slow release fertilizer is a chemical fertilizer which slowly releases available nutrients along with time through the chemical compound or physical action of the nutrients, and the release rate of the nutrients is far less than that of the nutrients which are converted into the available nutrients of plants after the quick soluble fertilizer is applied to soil. The coated slow-release fertilizer is a main slow-release fertilizer in the current market and can be divided into two types of inorganic coated fertilizers and organic polymer coated fertilizers according to different coating materials. The inorganic coated fertilizer has poor elasticity and is easy to be brittle, and the controlled release of nutrients cannot be realized; the organic coating material is difficult to degrade and is not beneficial to realizing environmental protection and plant growth, and some degradable coating materials cannot ensure the slow release process along with the expansion of coating pores and cannot control the release of nutrients. Therefore, a slow-release long-acting compound fertilizer for corn planting and a preparation method thereof are provided.
Disclosure of Invention
The invention aims to provide a slow-release long-acting compound fertilizer for corn planting and a preparation method thereof, and aims to solve the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme: the slow-release long-acting compound fertilizer for corn planting comprises a coating and a built-in fertilizer, wherein the coating comprises the following components in parts by weight: 30-42 parts of slow release resin, 20-36 parts of water-absorbent resin, 12-18 parts of inorganic salt and 1-5 parts of pullulan.
Further, the slow release resin comprises the following components: the composite material comprises starch, lignin, organic amine and epoxy chloropropane, wherein the mass ratio of the starch to the lignin is 1 (1-3.2).
Further, the water absorbent resin comprises the following components: polyglutamic acid, carbodiimide, N-hydroxysuccinimide ethylenediamine, 1, 6-hexamethylene diisocyanate, organic tin, hexanediol and amino-terminated polyethylene glycol.
Further, the built-in fertilizer comprises the following components in parts by weight: 6-10 parts of hydrotalcite, 9-18 parts of attapulgite, 6-9 parts of inorganic salt and 1.5-4.7 parts of glutamic acid.
Further, the inorganic salt is a soluble inorganic fertilizer, including a soluble nitrogenous fertilizer, a phosphate fertilizer, a potash fertilizer, a trace element fertilizer and the like.
A preparation method of a slow-release long-acting compound fertilizer for corn planting comprises the following steps:
(1) preparing water-absorbent resin:
adding carbodiimide and N-hydroxysuccinimide into polyglutamic acid, stirring and reacting in a nitrogen atmosphere, taking a product, adding a sodium bicarbonate solution and ethylenediamine, and reacting to obtain polyglutamic acid containing amino;
taking dimethylbenzene, slowly adding 1, 6-hexamethylene diisocyanate, heating in a nitrogen atmosphere, adding organic tin and hexanol, reacting at a constant temperature, adding hexanediol and organic tin, and continuing to react to obtain a polyurethane compound;
adding amino-terminated polyethylene glycol and a urethane compound into amino-containing polyglutamic acid, stirring, and reacting to obtain water-absorbent resin;
(2) preparing slow-release resin:
taking starch, adding epoxy chloropropane, mixing and stirring, heating, adding perchloric acid solution, reacting, filtering, washing, drying and sieving to obtain modified starch;
adding an alkaline solution into lignin, heating, washing, filtering, and drying to obtain pretreated lignin;
adding alkaline solution into the pretreated lignin, heating for reaction, adding epoxy chloropropane, reacting, cooling, filtering, washing and drying to obtain modified lignin;
blending modified starch and modified lignin, adding deionized water, stirring, adding organic amine, heating for reaction, filtering, washing, drying and sieving to obtain slow-release resin;
(3) preparing a built-in fertilizer:
dissolving inorganic salt in deionized water, adding glutamic acid, and stirring to obtain salt solution;
adding salt solution into pulvis Talci and attapulgite, pulverizing, mixing, pressing into balls, and drying to obtain built-in fertilizer;
(4) preparing a compound fertilizer:
dissolving water-absorbent resin in acetone, and adding aqueous solution of inorganic salt and pullulan to obtain water-absorbent resin mixed solution;
dissolving the slow-release resin in acetone, adding inorganic salt, stirring uniformly, immersing the built-in fertilizer in the slow-release resin, taking out, drying, immersing the built-in fertilizer in the water-absorbent resin mixed solution, taking out, drying to form a coating film, and preparing the compound fertilizer.
Further, the preparation of the water-absorbent resin comprises the following steps:
dissolving polyglutamic acid in water, adding carbodiimide EDC, stirring for dissolving, adding N-hydroxysuccinimide, stirring for reacting for 1-20 h in a nitrogen atmosphere, adding ethanol, filtering, drying, taking a product, adding a sodium bicarbonate solution, stirring and mixing, adding ethylenediamine, and reacting for 1-24 h to obtain the amino-containing polyglutamic acid;
taking dimethylbenzene, slowly adding 1, 6-hexamethylene diisocyanate, stirring in a nitrogen atmosphere, slowly heating to 78-82 ℃, slowly adding organic tin, stirring, slowly adding a dimethylbenzene solution of hexanol, reacting at a constant temperature, slowly adding hexanediol and organic tin when the hydroxyl content is close to 0, stirring in a nitrogen atmosphere, heating to 108-112 ℃, and keeping the temperature for 280-320 min to obtain a polyurethane compound;
and adding amino-terminated polyethylene glycol into amino-containing polyglutamic acid, dissolving in a mixed solvent of xylene and isobutanol, adjusting the temperature of the system to 0-3 ℃, adding a urethane compound, stirring, and reacting for 5-15 min to obtain the water-absorbent resin.
Further, the preparation of the slow-release resin comprises the following steps:
a. taking starch, adding epoxy chloropropane, mixing and stirring, heating to 95-100 ℃, adding a perchloric acid solution and sodium chloride, continuously reacting for 3-4 hours, filtering, washing, drying at 78-83 ℃ to constant weight, and sieving to obtain modified starch;
b. adding a sodium hydroxide solution into lignin, heating and boiling for 3-4 h, washing, carrying out suction filtration, and drying at 57-62 ℃ to constant weight to obtain pretreated lignin;
taking the pretreated lignin, adding a sodium hydroxide solution and toluene, heating to 118-122 ℃, reacting for 30-40 min, adding epoxy chloropropane, stirring at 118-122 ℃, reacting for 1-8 h, cooling to room temperature, performing suction filtration, washing, drying at 55-65 ℃ to constant weight, and sieving to obtain modified lignin;
c. and (2) blending modified starch and modified lignin, adding deionized water, stirring, adding organic amine, heating to 40-93 ℃, reacting for 3.5-7 h, filtering, washing, drying at 68-73 ℃ to constant weight, and sieving to obtain the slow-release resin.
Further, the molar ratio of hydroxyl in hexanol to isocyanate in 1, 6-hexamethylene diisocyanate is 1 (2-2.2);
the molar ratio of hydroxyl in the hexanediol to isocyanate in the 1, 6-hexamethylene diisocyanate is (1.0-1.1): 1.
Further, the mass ratio of the starch to the epoxy chloropropane in the step a is 1 (0.8-1), and the mass ratio of the lignin to the epoxy chloropropane in the step b is 1 (1-3.5).
In the technical scheme, amino is introduced into polyglutamic acid, a polyurethane compound prepared from diisocyanate, hexanol and hexanediol reacts with amino-terminated polyethylene glycol to prepare polyurethane-grafted polyglutamic acid and polyethylene glycol copolymer, the water absorption and degradation performance of the prepared water-absorbent resin can be improved while the properties of the polyglutamic acid and the polyethylene glycol are maintained, the shrinkage and expansion of the swelling volume under the acid-base condition are realized by using carboxyl of a side chain, the better water retention performance can be maintained under the alkaline soil environment, elements required by soil can be complexed, and the prepared compound fertilizer can provide more comprehensive nutrient supply for the soil; the elasticity and the strength of the water-absorbent resin are improved, and when the water-absorbent resin is coated on the outer surface of the built-in fertilizer, the prepared compound fertilizer is prevented from cracking, so that the problem that the nutrient release is out of control when the compound fertilizer is used due to the increase of transportation difficulty is avoided;
the starch and the lignin are modified by epoxy chloropropane, and then polymerized by organic amine to prepare the urethane grafted slow-release resin which has multiple pores, can adsorb inorganic salt, introduces nitrogen element, promotes the exchange between anions in soil and the prepared compound fertilizer, and realizes the release of nutrients and the adjustment of soil acidity and alkalinity; the capability of the prepared compound fertilizer for adsorbing and removing heavy metals can be improved, and the compound fertilizer has better heat resistance and acid and alkali resistance;
mixing hydrotalcite, attapulgite, inorganic salt and glutamic acid to prepare a built-in fertilizer, wherein the inorganic salt and the glutamic acid are inserted between hydrotalcite layers to achieve a slow release effect, and the attapulgite is bonded to compress the built-in fertilizer into balls;
finally, sequentially adding the built-in fertilizer into a slow-release resin solution containing inorganic salt and a water-absorbing resin mixed solution containing inorganic salt and pullulan, and coating by using a drum or high tower process, wherein the pullulan improves the adsorption capacity of the water-absorbing resin on the inorganic salt, and the prepared compound fertilizer is coated to prepare the compound fertilizer; wherein the inorganic salt components in the water-absorbent resin, the slow-release resin and the built-in fertilizer can be set according to the growth requirements of plants.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the compound fertilizer containing polyglutamic acid and the preparation method thereof, when the compound fertilizer is used, the inorganic salt is slowly released by the water-absorbing resin at the first stage, the water-absorbing resin is degraded at the second stage to expose the slow-release resin, the slow-release resin starts to degrade and release the inorganic salt, the slow-release resin is degraded at the third stage to form pores, the built-in fertilizer is exposed and flows out, and the controlled release of nutrients in the compound fertilizer is realized, wherein the inorganic salt components in the water-absorbing resin, the slow-release resin and the built-in fertilizer can be set according to different components according to the growth requirements of plants, so that the nutrient requirements of the plants at different growth stages are met, and the lasting and comprehensive nutrients are provided.
2. According to the compound fertilizer containing polyglutamic acid and the preparation method thereof, through the components of the water-absorbent resin and the arrangement of the preparation process thereof, the polyurethane compound is utilized to polymerize amino-containing polyglutamic acid and amino-terminated polyethylene glycol, the performances of the polyglutamic acid and the polyethylene glycol are retained, the water absorption and degradation performances of the prepared water-absorbent resin are improved, the water retention performance is exerted, the pH value of soil is adjusted, cations required by the soil are complexed, and the required anions are adsorbed, so that comprehensive nutrient supply is provided for the soil, the elasticity and the strength of the water-absorbent resin are improved.
3. According to the compound fertilizer containing polyglutamic acid and the preparation method thereof, through the arrangement of the components of the slow-release resin and the preparation process thereof, epichlorohydrin modified starch and lignin are polymerized by using organic amine to form the porous slow-release resin, so that inorganic salt is adsorbed, nitrogen is introduced, the exchange of anions in soil and the anions in the slow-release resin is promoted, and the release of nutrients and the adjustment of the acid-base property of the soil are realized; and the adsorption and heavy metal removal of the prepared compound fertilizer can be improved, and the compound fertilizer has better heat resistance and acid-base resistance.
4. According to the compound fertilizer containing polyglutamic acid and the preparation method thereof, the inorganic salt and the glutamic acid are arranged between hydrotalcite layers through the components of the built-in fertilizer and the preparation process thereof, so that the slow release effect is achieved, the attapulgite is bonded, and the built-in fertilizer is pressed into balls to prepare the built-in fertilizer, wherein the water-absorbent resin, the slow release resin and the glutamic acid are degraded when the prepared coated slow release resin is used, so that nitrogen elements are provided for soil, the performances of water absorption, degradation and the like of the prepared coated slow release resin are improved, the addition of a nitrogen fertilizer in the inorganic salt can be reduced, and the cost is reduced.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
(1) Preparing water-absorbent resin:
dissolving polyglutamic acid in water, adding carbodiimide EDC, stirring for dissolving, adding N-hydroxysuccinimide, stirring for reacting for 1h in a nitrogen atmosphere, adding ethanol, filtering, drying, taking a product, adding a sodium bicarbonate solution, stirring for mixing, adding ethylenediamine, and reacting for 1h to obtain polyglutamic acid containing amino;
taking dimethylbenzene, slowly adding 1, 6-hexamethylene diisocyanate, stirring in a nitrogen atmosphere, heating to 78 ℃, slowly adding organic tin, stirring, slowly adding a dimethylbenzene solution of hexanol, reacting at a constant temperature, slowly adding hexanediol and organic tin when the hydroxyl content is close to 0, stirring in a nitrogen atmosphere, heating to 108 ℃, and keeping the temperature for 280min to obtain a polyurethane compound; the molar ratio of the hydroxyl groups in hexanol to the isocyanate in 1, 6-hexamethylene diisocyanate is 1: 2; the molar ratio of hydroxyl in hexanediol to isocyanate in 1, 6-hexamethylene diisocyanate is 1: 1;
adding amino-terminated polyethylene glycol into amino-containing polyglutamic acid, dissolving in mixed solvent of xylene and isobutanol, adjusting the temperature of the system to 3 ℃, adding a urethane compound, stirring, and reacting for 5min to obtain water-absorbent resin;
(2) preparing slow-release resin:
taking starch and lignin for later use, wherein the mass of the starch is 10 parts, and the mass ratio of the starch to the lignin is 1: 1;
taking starch, adding epoxy chloropropane, mixing and stirring, heating to 95 ℃, adding a perchloric acid solution and sodium chloride, continuously reacting for 3 hours, filtering, washing, drying at 78 ℃ to constant weight, and sieving to obtain modified starch; the mass ratio of the starch to the epichlorohydrin is 1: 0.8;
adding a sodium hydroxide solution into lignin, heating and boiling for 3 hours, washing, carrying out suction filtration, and drying at 57 ℃ to constant weight to obtain pretreated lignin;
adding sodium hydroxide solution and toluene into pretreated lignin, heating to 118 ℃, reacting for 30min, adding epoxy chloropropane, stirring at 118 ℃, reacting for 1h, cooling to room temperature, performing suction filtration, washing, drying at 55 ℃ to constant weight, and sieving to obtain modified lignin; the mass ratio of the lignin to the epichlorohydrin is 1: 1;
mixing modified starch and modified lignin, adding deionized water, stirring, adding organic amine, heating to 40 deg.C, reacting for 3.5h, filtering, washing, drying at 68 deg.C to constant weight, and sieving to obtain sustained-release resin;
(3) preparing a built-in fertilizer:
taking the following components in parts by weight for later use: 6 parts of hydrotalcite, 9 parts of attapulgite, 6 parts of inorganic salt and 1.5 parts of glutamic acid, dissolving the inorganic salt in deionized water, adding the glutamic acid, and stirring to prepare a salt solution;
adding salt solution into pulvis Talci and attapulgite, pulverizing, mixing, pressing into balls, and drying to obtain built-in fertilizer;
(4) preparing a compound fertilizer:
taking the following components in parts by weight for later use: 30 parts of slow release resin, 20 parts of water-absorbent resin, 12 parts of inorganic salt and 1 part of pullulan, wherein the water-absorbent resin is dissolved in acetone, and aqueous solution of the inorganic salt and the pullulan are added to prepare water-absorbent resin mixed solution;
dissolving the slow-release resin in acetone, adding inorganic salt, stirring uniformly, immersing the built-in fertilizer in the slow-release resin, taking out, drying, immersing the built-in fertilizer in the water-absorbent resin mixed solution, taking out, drying to form a coating film, and preparing the compound fertilizer.
Example 2
(1) Preparing water-absorbent resin:
dissolving polyglutamic acid in water, adding carbodiimide EDC, stirring for dissolving, adding N-hydroxysuccinimide, stirring for reacting for 10h in a nitrogen atmosphere, adding ethanol, filtering, drying, taking a product, adding a sodium bicarbonate solution, stirring for mixing, adding ethylenediamine, and reacting for 12h to obtain polyglutamic acid containing amino;
taking dimethylbenzene, slowly adding 1, 6-hexamethylene diisocyanate, stirring in a nitrogen atmosphere, heating to 80 ℃, slowly adding organic tin, stirring, slowly adding a dimethylbenzene solution of hexanol, reacting at a constant temperature, slowly adding hexanediol and organic tin when the hydroxyl content is close to 0, stirring in a nitrogen atmosphere, heating to 110 ℃, and keeping the temperature for 300min to obtain a polyurethane compound; the molar ratio of the hydroxyl groups in hexanol to the isocyanate in 1, 6-hexamethylene diisocyanate was 1: 2.1; the molar ratio of hydroxyl in hexanediol to isocyanate in 1, 6-hexamethylene diisocyanate is 1.05: 1;
adding amino-terminated polyethylene glycol into amino-containing polyglutamic acid, dissolving in mixed solvent of xylene and isobutanol, adjusting the temperature of the system to 1 ℃, adding a urethane compound, stirring, and reacting for 10min to obtain water-absorbent resin;
(2) preparing slow-release resin:
taking starch and lignin for later use, wherein the mass of the starch is 10 parts, and the mass ratio of the starch to the lignin is 1: 2.2;
taking starch, adding epoxy chloropropane, mixing and stirring, heating to 98 ℃, adding a perchloric acid solution and sodium chloride, continuously reacting for 3.5h, filtering, washing, drying at 80 ℃ to constant weight, and sieving to obtain modified starch; the mass ratio of the starch to the epichlorohydrin is 1: 0.9;
adding a sodium hydroxide solution into lignin, heating and boiling for 3.5h, washing, carrying out suction filtration, and drying at 60 ℃ to constant weight to obtain pretreated lignin;
taking the pretreated lignin, adding a sodium hydroxide solution and toluene, heating to 120 ℃, reacting for 35min, adding epoxy chloropropane, stirring and reacting for 4.5h at 120 ℃, cooling to room temperature, carrying out suction filtration, washing, drying at 60 ℃ to constant weight, and sieving to obtain modified lignin; the mass ratio of the lignin to the epichlorohydrin is 1: 2.2;
mixing modified starch and modified lignin, adding deionized water, stirring, adding organic amine, heating to 66 deg.C, reacting for 5.7h, filtering, washing, drying at 70 deg.C to constant weight, and sieving to obtain sustained-release resin;
(3) preparing a built-in fertilizer:
taking the following components in parts by weight for later use: 8 parts of hydrotalcite, 14 parts of attapulgite, 7 parts of inorganic salt and 3.1 parts of glutamic acid, dissolving the inorganic salt in deionized water, adding the glutamic acid, and stirring to prepare a salt solution;
adding salt solution into pulvis Talci and attapulgite, pulverizing, mixing, pressing into balls, and drying to obtain built-in fertilizer;
(4) preparing a compound fertilizer:
taking the following components in parts by weight for later use: 36 parts of slow release resin, 28 parts of water-absorbent resin, 15 parts of inorganic salt and 3 parts of pullulan, wherein the water-absorbent resin is dissolved in acetone, and an aqueous solution of the inorganic salt and the pullulan are added to prepare a water-absorbent resin mixed solution;
dissolving the slow-release resin in acetone, adding inorganic salt, stirring uniformly, immersing the built-in fertilizer in the slow-release resin, taking out, drying, immersing the built-in fertilizer in the water-absorbent resin mixed solution, taking out, drying to form a coating film, and preparing the compound fertilizer.
Example 3
(1) Preparing water-absorbent resin:
dissolving polyglutamic acid in water, adding carbodiimide EDC, stirring for dissolving, adding N-hydroxysuccinimide, stirring for reacting for 20h in a nitrogen atmosphere, adding ethanol, filtering, drying, taking a product, adding a sodium bicarbonate solution, stirring for mixing, adding ethylenediamine, and reacting for 24h to obtain polyglutamic acid containing amino;
taking dimethylbenzene, slowly adding 1, 6-hexamethylene diisocyanate, stirring in a nitrogen atmosphere, heating to 82 ℃, slowly adding organic tin, stirring, slowly adding a dimethylbenzene solution of hexanol, reacting at a constant temperature, slowly adding hexanediol and organic tin when the hydroxyl content is close to 0, stirring in a nitrogen atmosphere, heating to 112 ℃, and keeping the temperature for 320min to obtain a polyurethane compound; the molar ratio of the hydroxyl groups in hexanol to the isocyanate in 1, 6-hexamethylene diisocyanate was 1: 2.2; the molar ratio of hydroxyl in hexanediol to isocyanate in 1, 6-hexamethylene diisocyanate is 1.1: 1;
adding amino-terminated polyethylene glycol into amino-containing polyglutamic acid, dissolving in mixed solvent of xylene and isobutanol, adjusting the temperature of the system to 0 ℃, adding a urethane compound, stirring, and reacting for 15min to obtain water-absorbent resin;
(2) preparing slow-release resin:
taking starch and lignin for later use, wherein the mass of the starch is 10 parts, and the mass ratio of the starch to the lignin is 1: 3.2;
taking starch, adding epoxy chloropropane, mixing and stirring, heating to 100 ℃, adding a perchloric acid solution and sodium chloride, continuously reacting for 4 hours, filtering, washing, drying at 83 ℃ to constant weight, and sieving to obtain modified starch; the mass ratio of the starch to the epichlorohydrin is 1: 1;
adding a sodium hydroxide solution into lignin, heating and boiling for 3-4 h, washing, carrying out suction filtration, and drying at 62 ℃ to constant weight to obtain pretreated lignin;
taking the pretreated lignin, adding a sodium hydroxide solution and toluene, heating to 122 ℃, reacting for 40min, adding epoxy chloropropane, stirring at 122 ℃, reacting for 1-8 h, cooling to room temperature, performing suction filtration, washing, drying at 65 ℃ to constant weight, and sieving to obtain modified lignin; the mass ratio of the lignin to the epichlorohydrin is 1: 3.5;
blending modified starch and modified lignin, adding deionized water, stirring, adding organic amine, heating to 93 deg.C, reacting for 7h, filtering, washing, drying at 73 deg.C to constant weight, and sieving to obtain sustained-release resin;
(3) preparing a built-in fertilizer:
taking the following components in parts by weight for later use: 10 parts of hydrotalcite, 18 parts of attapulgite, 9 parts of inorganic salt and 4.7 parts of glutamic acid, dissolving the inorganic salt in deionized water, adding the glutamic acid, and stirring to prepare a salt solution;
adding salt solution into pulvis Talci and attapulgite, pulverizing, mixing, pressing into balls, and drying to obtain built-in fertilizer;
(4) preparing a compound fertilizer:
taking the following components in parts by weight for later use: 42 parts of slow release resin, 36 parts of water-absorbent resin, 18 parts of inorganic salt and 5 parts of pullulan, wherein the water-absorbent resin is dissolved in acetone, and aqueous solution of the inorganic salt and the pullulan are added to prepare water-absorbent resin mixed solution;
dissolving the slow-release resin in acetone, adding inorganic salt, stirring uniformly, immersing the built-in fertilizer in the slow-release resin, taking out, drying, immersing the built-in fertilizer in the water-absorbent resin mixed solution, taking out, drying to form a coating film, and preparing the compound fertilizer.
Comparative example 1
(1) Preparing water-absorbent resin:
taking dimethylbenzene, slowly adding 1, 6-hexamethylene diisocyanate, stirring in a nitrogen atmosphere, heating to 80 ℃, slowly adding organic tin, stirring, slowly adding a dimethylbenzene solution of hexanol, reacting at a constant temperature, slowly adding hexanediol and organic tin when the hydroxyl content is close to 0, stirring in a nitrogen atmosphere, heating to 110 ℃, and keeping the temperature for 300min to obtain a polyurethane compound; the molar ratio of the hydroxyl groups in hexanol to the isocyanate in 1, 6-hexamethylene diisocyanate was 1: 2.1; the molar ratio of hydroxyl in hexanediol to isocyanate in 1, 6-hexamethylene diisocyanate is 1.05: 1;
adding polyethylene glycol into polyglutamic acid, dissolving in mixed solvent of xylene and isobutanol, adjusting the temperature of the system to 1 ℃, adding a urethane compound, and stirring to obtain water-absorbent resin;
the other steps and implementation parameters were identical to those of example 2.
Comparative example 2
(2) Preparing slow-release resin:
mixing starch and lignin, adding deionized water, stirring, filtering, washing, drying at 70 deg.C to constant weight, and sieving to obtain sustained-release resin; wherein the mass ratio of starch to lignin is 1: 2.2;
the other steps and implementation parameters were identical to those of example 2.
Comparative example 3
(1) Preparing a built-in fertilizer:
taking the following components in parts by weight for later use: 8 parts of hydrotalcite, 14 parts of attapulgite, 7 parts of inorganic salt and 3.1 parts of glutamic acid, dissolving the inorganic salt in deionized water, adding the glutamic acid, and stirring to prepare a salt solution;
adding salt solution into pulvis Talci and attapulgite, pulverizing, mixing, pressing into balls, and drying to obtain built-in fertilizer;
(2) preparing a compound fertilizer:
preparing a solution from polyglutamic acid, immersing the built-in fertilizer in the solution, taking out the solution, and drying to form a coating film to prepare the compound fertilizer.
The inorganic salt is a mixture of soluble nitrogenous fertilizer, phosphate fertilizer, potash fertilizer and trace element fertilizer, and the components and the proportion are the same in each embodiment and comparative example.
Experiment of
Taking the compound fertilizers obtained in the examples 1-3 and the comparative examples 1-3 to prepare samples, respectively detecting the water retention performance and the fertilizer slow release performance of the samples, and recording the detection results:
and (4) testing the water retention performance: taking two groups of beakers, and adding 100g of dry soil and 200g of deionized water into one group of beakers to serve as a blank group; 2g of sample, 100g of dry soil and 200g of deionized water are added into the two groups, the mixture is placed at room temperature and continuously observed for 20 days, and the water loss rate in a beaker is taken as a water retention performance index;
and (3) testing slow release performance of the fertilizer: taking 1g of sample, placing the sample in 500g of deionized water and 500g of dry soil, placing the sample at a constant temperature of 25 ℃, testing the nitrogen content in the solution at different time periods, wherein the nitrogen content is determined by a Kjeldahl semi-micro nitrogen determination method, thus obtaining the release speed of the nitrogen element, and taking the ratio of the nitrogen element content in the solution to the nitrogen element content in the sample as a slow release rate which is used as a slow release index of the fertilizer.
From the data in the table above, it is clear that the following conclusions can be drawn:
the compound fertilizers obtained in the examples 1-3 are compared with the compound fertilizers obtained in the comparative examples 1-3, and the detection results show that,
1. compared with the compound fertilizer and the blank group obtained in the comparative example 3, the compound fertilizer obtained in the examples 1-3 has the advantages that the water loss rate data is obviously reduced, and the rising rate of the slow release rate data at the initial stage is obviously slowed, which fully shows that the water retention performance and the fertilizer slow release performance of the compound fertilizer prepared by the invention are improved;
the implementation parameters in examples 1-3 are different, and the implementation parameters are always kept at a better level compared with comparative examples 1-3 and a blank group, so that the prepared compound fertilizer can be kept to have better water retention performance and fertilizer slow release performance within the implementation process and implementation parameter range of the invention;
2. the water absorbent resin in comparative example 1 was prepared differently compared to example 2; the preparation of the slow release resin in comparative example 2 was different; the coating in the compound fertilizer in the comparative example 3 is polyglutamic acid, the water loss rate and slow release rate data of which are obviously changed, and the components and the preparation process thereof can promote the water retention performance and the slow release performance of the prepared compound fertilizer.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Furthermore, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process method article or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process method article or apparatus.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement and improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A slow-release long-acting compound fertilizer for corn planting is characterized in that: the fertilizer comprises a coating and a built-in fertilizer, wherein the coating comprises the following components in parts by weight: 30-42 parts of slow release resin, 20-36 parts of water-absorbent resin, 12-18 parts of inorganic salt and 1-5 parts of pullulan.
2. The slow-release long-acting compound fertilizer for corn planting according to claim 1, characterized in that: the slow release resin comprises the following components: the composite material comprises starch, lignin, organic amine and epoxy chloropropane, wherein the mass ratio of the starch to the lignin is 1 (1-3.2).
3. The slow-release long-acting compound fertilizer for corn planting according to claim 1, characterized in that: the water-absorbent resin comprises the following components: polyglutamic acid, carbodiimide, N-hydroxysuccinimide ethylenediamine, 1, 6-hexamethylene diisocyanate, organotin, hexanol, hexanediol, amino-terminated polyethylene glycol.
4. The slow-release long-acting compound fertilizer for corn planting and the preparation method thereof according to claim 1, wherein the slow-release long-acting compound fertilizer comprises the following components: the built-in fertilizer comprises the following components in parts by weight: 6-10 parts of hydrotalcite, 9-18 parts of attapulgite, 6-9 parts of inorganic salt and 1.5-4.7 parts of glutamic acid.
5. The slow-release long-acting compound fertilizer for corn planting according to claim 4, wherein the slow-release long-acting compound fertilizer comprises the following components in parts by weight: the inorganic salt is a soluble inorganic fertilizer.
6. A preparation method of a slow-release long-acting compound fertilizer for corn planting is characterized by comprising the following steps: the method comprises the following steps:
(1) preparing water-absorbent resin:
adding carbodiimide and N-hydroxysuccinimide into polyglutamic acid, stirring and reacting in a nitrogen atmosphere, taking a product, adding a sodium bicarbonate solution and ethylenediamine, and reacting to obtain polyglutamic acid containing amino;
taking dimethylbenzene, slowly adding 1, 6-hexamethylene diisocyanate, slowly controlling temperature rise in a nitrogen atmosphere, adding organic tin and hexanol, reacting at constant temperature, adding hexanediol and organic tin, and continuing to react to obtain a polyurethane compound;
adding amino-terminated polyethylene glycol into amino-containing polyglutamic acid, adding a urethane compound, stirring, and reacting to obtain water-absorbent resin;
(2) preparing slow-release resin:
taking starch, adding epoxy chloropropane, mixing and stirring, heating, adding perchloric acid solution, reacting, filtering, washing, drying and sieving to obtain modified starch;
adding an alkaline solution into lignin, heating, washing, filtering, and drying to obtain pretreated lignin;
adding alkaline solution into the pretreated lignin, heating for reaction, adding epoxy chloropropane, reacting, cooling, filtering, washing and drying to obtain modified lignin;
blending modified starch and modified lignin, adding deionized water, stirring, adding organic amine, heating for reaction, filtering, washing, drying and sieving to obtain slow-release resin;
(3) preparing a built-in fertilizer:
dissolving inorganic salt in deionized water, adding glutamic acid, and stirring to obtain salt solution;
adding salt solution into pulvis Talci and attapulgite, pulverizing, mixing, pressing into balls, and drying to obtain built-in fertilizer;
(4) preparing a compound fertilizer:
dissolving water-absorbent resin in acetone, and adding aqueous solution of inorganic salt and pullulan to obtain water-absorbent resin mixed solution;
dissolving the slow-release resin in acetone, adding inorganic salt, stirring uniformly, immersing the built-in fertilizer in the slow-release resin, taking out, drying, immersing the built-in fertilizer in the water-absorbent resin mixed solution, taking out, drying to form a coating film, and preparing the compound fertilizer.
7. The method for preparing the slow-release long-acting compound fertilizer for corn planting according to claim 6, characterized in that: the preparation of the water-absorbent resin comprises the following steps:
dissolving polyglutamic acid in water, adding carbodiimide EDC, stirring for dissolving, adding N-hydroxysuccinimide, stirring for reacting for 1-20 h in a nitrogen atmosphere, adding ethanol, filtering, drying, taking a product, adding a sodium bicarbonate solution, stirring and mixing, adding ethylenediamine, and reacting for 1-24 h to obtain the amino-containing polyglutamic acid;
taking dimethylbenzene, slowly adding 1, 6-hexamethylene diisocyanate, stirring in a nitrogen atmosphere, slowly heating to 78-82 ℃, slowly adding organic tin, stirring, slowly adding a dimethylbenzene solution of hexanol, reacting at a constant temperature, slowly adding hexanediol and organic tin when the hydroxyl content is close to 0, stirring in a nitrogen atmosphere, heating to 108-112 ℃, and keeping the temperature for 280-320 min to obtain a polyurethane compound;
and adding amino-terminated polyethylene glycol into amino-containing polyglutamic acid, dissolving in a mixed solvent of xylene and isobutanol, adjusting the temperature of the system to 0-3 ℃, adding a urethane compound, stirring, and reacting for 5-15 min to obtain the water-absorbent resin.
8. The method for preparing the slow-release long-acting compound fertilizer for corn planting according to claim 6, characterized in that: the preparation of the slow-release resin comprises the following steps:
a. taking starch, adding epoxy chloropropane, mixing and stirring, heating to 95-100 ℃, adding a perchloric acid solution and sodium chloride, continuously reacting for 3-4 hours, filtering, washing, drying at 78-83 ℃ to constant weight, and sieving to obtain modified starch;
b. adding a sodium hydroxide solution into lignin, heating and boiling for 3-4 h, washing, carrying out suction filtration, and drying at 57-62 ℃ to constant weight to obtain pretreated lignin;
taking the pretreated lignin, adding a sodium hydroxide solution and toluene, heating to 118-122 ℃, reacting for 30-40 min, adding epoxy chloropropane, stirring at 118-122 ℃, reacting for 1-8 h, cooling to room temperature, performing suction filtration, washing, drying at 55-65 ℃ to constant weight, and sieving to obtain modified lignin;
c. and (2) blending modified starch and modified lignin, adding deionized water, stirring, adding organic amine, heating to 40-93 ℃, reacting for 3.5-7 h, filtering, washing, drying at 68-73 ℃ to constant weight, and sieving to obtain the slow-release resin.
9. The method for preparing the slow-release long-acting compound fertilizer for corn planting according to claim 7, characterized in that: the molar ratio of hydroxyl in hexanol to isocyanate in 1, 6-hexamethylene diisocyanate is 1 (2-2.2); the molar ratio of hydroxyl in the hexanediol to isocyanate in the 1, 6-hexamethylene diisocyanate is (1.0-1.1): 1.
10. The method for preparing the slow-release long-acting compound fertilizer for corn planting according to claim 8, characterized in that: the mass ratio of the starch to the epoxy chloropropane in the step a is 1 (0.8-1), and the mass ratio of the lignin to the epoxy chloropropane in the step b is 1 (1-3.5).
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