CN114890841A - Long-acting microbial compound fertilizer and preparation method thereof - Google Patents
Long-acting microbial compound fertilizer and preparation method thereof Download PDFInfo
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- CN114890841A CN114890841A CN202210293416.1A CN202210293416A CN114890841A CN 114890841 A CN114890841 A CN 114890841A CN 202210293416 A CN202210293416 A CN 202210293416A CN 114890841 A CN114890841 A CN 114890841A
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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
- C05B—PHOSPHATIC FERTILISERS
- C05B7/00—Fertilisers based essentially on alkali or ammonium orthophosphates
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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
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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
- C05G5/00—Fertilisers characterised by their form
- C05G5/10—Solid or semi-solid fertilisers, e.g. powders
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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Abstract
The invention discloses a long-acting microbial compound fertilizer, which adopts modified porous polymer to adsorb microbes, carries out the first-step slow-release treatment, and in addition, adds a slow-release reinforcing agent in an embedding liquid as the second-step slow-release treatment, thereby effectively inhibiting the agglomeration phenomenon of the modified porous polymer, providing necessary nutrient substances for slow-release bacterial liquid, promoting the propagation of microbial bacteria, ensuring the sufficient nutrient supply of the whole growth cycle of crops, and improving the utilization rate of the fertilizer. The long-acting microbial compound fertilizer provided by the invention is simple to prepare and convenient to use, can obviously improve the soil microenvironment after being used, and cannot cause secondary pollution to the soil.
Description
Technical Field
The invention belongs to the technical field of fertilizers, and particularly relates to a long-acting microbial compound fertilizer and a preparation method thereof.
Background
China is a big country for agricultural development, the annual fertilizer application amount accounts for 35% of the total world amount, but the utilization rate of the fertilizer is far lower than that of developed countries, wherein the utilization rate of nitrogenous fertilizers is 30% -50%, the utilization rate of phosphatic fertilizers is 8% -20%, and the utilization rate of potash fertilizers is about 50%. The utilization rate of the fertilizer is improved, the economic pressure of agricultural planting can be reduced, and the pollution to the environment can be reduced. Development of a controlled release fertilizer is an important approach to solve this problem.
Microbial fertilizers are mainly completed by the life activities of a large number of beneficial microorganisms contained in the microbial fertilizer. At present, the microbial fertilizer in China develops rapidly, the variety is increased continuously, but the microbial fertilizer has the defects of unstable fertilizer efficiency, easy influence of environmental factors and the like. The addition of microorganisms mostly stays in the direct addition of microbial powder, microbial strains are exposed in the external environment and are easily inactivated by the influence of temperature, pH and salt in the production and use processes, and in addition, the powder and granular fertilizer are easy to run off when being applied together and cannot be effectively combined with soil, so that the number of viable bacteria of the biological microbial inoculum actually entering the soil is small or the activity of the biological microbial inoculum is too low, and the due efficacy of the biological microbial inoculum cannot be exerted.
Chinese patent CN 113354470A discloses a composite microorganism slow-release bacterial fertilizer and a preparation method thereof, comprising the following steps of firstly, preparing bacterial suspension of aspergillus oryzae and bacterial suspension of bacillus mucilaginosus; step two, adding the bacterial suspension of aspergillus oryzae and the chemical fertilizer into the first mixed colloid, and uniformly mixing to obtain a second mixed colloid; adding the bacterial suspension of the bacillus mucilaginosus and the chemical fertilizer into the first mixed colloid, and uniformly mixing to obtain a third mixed colloid; wherein, the first mixed colloid is obtained by sterilizing a solution containing an adsorbent, a nutrient substance and an embedding agent under high pressure and cooling to room temperature; step three, adding the second mixed colloid into a cross-linking agent for cross-linking and fixing, and drying to obtain first compound fertilizer particles; adding the third mixed colloid into a cross-linking agent for cross-linking and fixing, and drying to obtain second compound fertilizer particles; and step four, mixing the first compound fertilizer particles and the second compound fertilizer particles to obtain the compound microorganism slow-release bacterial fertilizer. The invention realizes better sustained-release effect, however, the demand of the plant growth process on nutrient substances often presents an S curve, and the situation of insufficient or excessive nutrient supply may occur during the sustained-release period, which is not beneficial to the growth of crops and the full utilization of fertilizer efficiency.
Disclosure of Invention
Aiming at the defects of the existing microbial fertilizer, the invention provides a long-acting microbial compound fertilizer and a preparation method thereof.
A preparation method of a long-acting microbial compound fertilizer comprises the following steps:
according to the mass parts, 40-50 parts of embedding liquid is taken by an injector with the caliber of 1-2 mm, the embedding liquid is dripped into 100-120 parts of stationary liquid according to the dripping speed of 3-5 mL/min, the mixture is solidified for 1-3 h at the rotating speed of 60-80 rpm and then filtered to obtain a solidified substance, and the solidified substance is washed by water and naturally dried at the temperature of 25-35 ℃ to obtain the long-acting microbial compound fertilizer.
The preparation method of the embedding liquid comprises the following steps:
according to the mass parts, 8-10 parts of modified porous polymer, 10-15 parts of sodium alginate and 12-14 parts of slow release reinforcing agent are added into 100-120 parts of water, the mixture is stirred at 45-55 ℃ and 100-200 rpm for 10-15 min, then sterilized at 100-110 ℃ for 20-30 min, cooled to room temperature, 10-15 parts of microbial liquid and 30-40 parts of potassium dihydrogen phosphate are added, and the mixture is stirred at 100-200 rpm for 15-25 min to obtain the embedding liquid.
The preparation method of the modified porous polymer comprises the following steps:
t1: adding 1-2 parts by mass of melamine and 4-6 parts by mass of p-aldehyde benzoic acid into 50-60 parts by mass of o-xylene, condensing and refluxing for 8-10 h at 155-165 ℃, cooling to room temperature, performing suction filtration to obtain a filter cake A, and performing vacuum drying on the filter cake A for 8-10 h at 70-80 ℃ to obtain a ligand;
t2: adding 3-5 parts by mass of a ligand obtained in T1, 2-4 parts by mass of cobalt nitrate hexahydrate and 1-3 parts by mass of stannic chloride dihydrate into 50-60 parts by mass of a mixed solution, putting the mixed solution into a reaction kettle, reacting at 120-140 ℃ for 36-48 h, cooling to room temperature, performing suction filtration to obtain a filter cake B, and performing vacuum drying on the filter cake B at 70-80 ℃ for 8-10 h to obtain a porous polymer, wherein the mixed solution is prepared by mixing N, N-dimethylformamide and ethylenediamine according to a mass ratio of 1 (1-2);
t3: mixing the porous polymer obtained in the step T2 and Li 2 CO 3 、La 2 O 3 Mixing the raw materials according to a mass ratio of (4-6): 1- (1-3), uniformly grinding to obtain mixed powder I, flatly spreading the mixed powder I in a ceramic crucible with a cover, then placing the ceramic crucible in a muffle furnace at an initial temperature of 20-25 ℃, a heating rate of 2-4 ℃/min, a heating temperature of 170-200 ℃, and a temperature of 170 ℃ Calcining for 1.5-2.5 hours at 200 ℃ to obtain the modified porous polymer.
The slow release reinforcing agent is at least one of hydroxymethyl cellulose, sodium hydroxymethyl cellulose, lignin and sodium lignosulfonate; preferably, the slow-release reinforcing agent is prepared by mixing hydroxymethyl cellulose and sodium lignin sulfonate according to the mass ratio of 1 (1.5-2.5).
The embedding liquid is added with a modified porous polymer, wherein the porous polymer takes a reaction product of melamine and p-aldehyde benzoic acid as a ligand, and generates a space network structure by a complex reaction with zinc ions and cobalt ions, so that abundant storage sites are provided for the microbial liquid, and the porous polymer is Li 2 CO 3 And La 2 O 3 The modified porous polymer is obtained after composite modification, the appropriate band gap value of the modified porous polymer can well absorb ultraviolet rays, the activity of microbial bacteria stored in the modified porous polymer is improved, meanwhile, electron transition is excited, a hole with oxidizing capability is generated, harmful substances in soil are decomposed, and the soil is further purified.
However, the modified porous polymer is easy to generate spontaneous polymerization, so that the stored microbial thallus is unevenly released, in order to solve the problems, the inventor adds a slow release reinforcing agent into an embedding solution, wherein the slow release reinforcing agent is formed by mixing hydroxymethyl cellulose and sodium lignosulfonate, the sodium lignosulfonate contains active groups such as hydroxyl, carboxyl, methoxyl and the like, the active groups are closely related to the modified porous polymer through the action of hydrogen bonds, a three-dimensional net-shaped space structure is formed on the surface of the modified porous polymer, and the polymerization phenomenon of the modified porous polymer can be effectively avoided due to the electrostatic repulsion force caused by the electrification property of the modified porous polymer; the hydroxymethyl cellulose has good thickening effect, can reduce the agglomeration phenomenon of the modified porous polymer to a certain extent, and has good water retention effect. After the hydroxymethyl cellulose and the sodium lignosulfonate act together, the sodium lignosulfonate can strengthen the interaction between the hydroxymethyl cellulose to form an interpenetrating network structure, so that the mechanical stability of the microbial carrier is improved, and a better slow-release effect is obtained.
The preparation method of the microbial liquid comprises the following steps:
culturing the thawed Bacillus subtilis, Bacillus megaterium and azotobacter chroococcum by conventional culture method, respectively, and diluting the cultured bacteria liquid to the same concentration of 1 × 10 7 ～1×10 8 Obtaining a diluent after cfu/mL, and mixing the bacillus subtilis diluent, the bacillus megaterium diluent and the azotobacter chroococcum diluent according to the mass ratio of 1 (2-4): (1-3) mixing to obtain the microbial liquid.
The bacillus subtilis, the bacillus megaterium and the azotobacter chroococcum are reasonably matched as microbial fertilizers and are matched with the growth of crops for slow release, nutrient substances in soil and nitrogen elements in fixed air can be fully utilized, sufficient nutrient substances are provided for the growth of the crops, organic matters in the soil can be promoted to be decomposed into humic acid, the nutrient substances which cannot be directly absorbed by the crops in the soil are converted into the nutrient substances which can be directly utilized by the crops, the microbial content in the soil is improved, the soil quality is improved, and the quality guarantee and yield increase of the crops are realized.
The preparation method of the fixing liquid comprises the following steps:
according to the mass parts, 8-12 parts of calcium chloride and 25-30 parts of boric acid are added into 100-120 parts of water and uniformly stirred to obtain the stationary liquid.
The invention has the beneficial effects that:
(1) according to the long-acting microbial compound fertilizer prepared by the invention, microbes are fixed in the porous polymer, the abundant space network structure provides abundant storage sites for microbial liquid, the modified porous polymer can well absorb ultraviolet rays as a first step of slow release treatment, the activity of the stored microbial liquid in the porous polymer is improved, meanwhile, electron transition is excited, a hole with oxidation capacity is generated, harmful substances in soil are decomposed, and the soil is further purified.
(2) The long-acting microbial compound fertilizer provided by the invention is simple to prepare and convenient to use, can obviously improve the soil microenvironment after being used, and cannot cause secondary pollution to the soil.
Detailed Description
The raw materials used in the examples are as follows:
bacillus subtilis, latin name: bacillus subtilis, number: ACCC 60429, purchased from China agricultural microbial culture Collection management center.
Bacillus megaterium, latin name: bacillus megaterium, accession number: CICC 20665, purchased from China center for culture Collection of Industrial microorganisms.
Azotobacter chroococcum, name of latin: azotobacter chlorococcus, number: CICC 22661, purchased from China center for Industrial culture Collection of microorganisms.
Example 1
A preparation method of a long-acting microbial compound fertilizer comprises the following steps:
according to the mass parts, 40 parts of embedding liquid is taken by an injector with the caliber of 2mm, the embedding liquid is dripped into 100 parts of fixing liquid at the dripping speed of 5mL/min, the fixing liquid is solidified for 2 hours at the rotating speed of 60rpm and then filtered to obtain a solidified substance, and the solidified substance is washed by water for 3 times and then naturally dried at the temperature of 30 ℃ to obtain the long-acting microbial compound fertilizer.
The preparation method of the embedding liquid comprises the following steps:
adding 8 parts of modified porous polymer and 15 parts of sodium alginate into 120 parts of water according to parts by mass, stirring at 50 ℃ and 100rpm for 10min, sterilizing at 110 ℃ for 30min, cooling to room temperature, adding 10 parts of microbial liquid and 30 parts of potassium dihydrogen phosphate, and continuously stirring at 100rpm for 15min to obtain the embedding liquid.
The preparation method of the modified porous polymer comprises the following steps:
t1: adding 2 parts of melamine and 6 parts of p-aldehyde benzoic acid into 50 parts of o-xylene according to parts by mass, condensing and refluxing for 10 hours at 155 ℃, cooling to room temperature, performing suction filtration to obtain a filter cake A, and performing vacuum drying on the filter cake A for 10 hours at 80 ℃ to obtain a ligand;
t2: adding 3 parts by mass of ligand obtained in T1, 3 parts by mass of cobalt nitrate hexahydrate and 2 parts by mass of stannic chloride dihydrate into 50 parts by mass of mixed solution, putting into a reaction kettle, reacting at 120 ℃ for 48 hours, cooling to room temperature, carrying out suction filtration to obtain a filter cake B, and carrying out vacuum drying on the filter cake B at 80 ℃ for 10 hours to obtain a porous polymer, wherein the mixed solution is prepared by mixing N, N-dimethylformamide and ethylenediamine according to a mass ratio of 1: 1;
T3: mixing the porous polymer obtained in the step T2 and Li 2 CO 3 、La 2 O 3 Mixing the materials according to a mass ratio of 4:1:2, grinding the materials uniformly to obtain mixed powder I, spreading the mixed powder I in a ceramic crucible with a cover, then placing the ceramic crucible in a muffle furnace, wherein the initial temperature is 25 ℃, the heating rate is 3 ℃/min, the temperature is increased to 180 ℃, and the mixture is calcined for 2 hours at 180 ℃ to obtain the modified porous polymer.
The preparation method of the microbial liquid comprises the following steps:
culturing the thawed Bacillus subtilis, Bacillus megaterium and azotobacter chroococcum by conventional culture method, respectively, and diluting the cultured bacteria liquid to concentration of 1 × 10 8 Obtaining a diluent after cfu/mL, and mixing the bacillus subtilis diluent, the bacillus megaterium diluent and the azotobacter chroococcum diluent according to the mass ratio of 1:3:2 to obtain the microbial solution.
The preparation method of the fixing liquid comprises the following steps:
according to the mass parts, 10 parts of calcium chloride and 30 parts of boric acid are added into 100 parts of water and stirred uniformly to obtain the stationary liquid.
Example 2
A preparation method of a long-acting microbial compound fertilizer comprises the following steps:
according to the mass parts, 40 parts of embedding liquid is taken by an injector with the caliber of 2mm, the embedding liquid is dripped into 100 parts of fixing liquid at the dripping speed of 5mL/min, the fixing liquid is solidified for 2 hours at the rotating speed of 60rpm and then filtered to obtain a solidified substance, and the solidified substance is washed by water for 3 times and then naturally dried at the temperature of 30 ℃ to obtain the long-acting microbial compound fertilizer.
The preparation method of the embedding liquid comprises the following steps:
adding 8 parts by mass of modified porous polymer, 15 parts by mass of sodium alginate and 13 parts by mass of slow-release reinforcing agent into 120 parts by mass of water, stirring at 50 ℃ and 100rpm for 10min, sterilizing at 110 ℃ for 30min, cooling to room temperature, adding 10 parts by mass of microbial solution and 30 parts by mass of potassium dihydrogen phosphate, and continuously stirring at 100rpm for 15min to obtain the embedding solution.
The preparation method of the modified porous polymer comprises the following steps:
t1: adding 2 parts of melamine and 6 parts of p-aldehyde benzoic acid into 50 parts of o-xylene according to parts by mass, condensing and refluxing for 10 hours at 155 ℃, cooling to room temperature, performing suction filtration to obtain a filter cake A, and performing vacuum drying on the filter cake A for 10 hours at 80 ℃ to obtain a ligand;
t2: adding 3 parts by mass of ligand obtained in T1, 3 parts by mass of cobalt nitrate hexahydrate and 2 parts by mass of stannic chloride dihydrate into 50 parts by mass of mixed solution, putting into a reaction kettle, reacting at 120 ℃ for 48 hours, cooling to room temperature, carrying out suction filtration to obtain a filter cake B, and carrying out vacuum drying on the filter cake B at 80 ℃ for 10 hours to obtain a porous polymer, wherein the mixed solution is prepared by mixing N, N-dimethylformamide and ethylenediamine according to a mass ratio of 1: 1;
t3: mixing the porous polymer obtained in the step T2 and Li 2 CO 3 、La 2 O 3 Mixing the materials according to a mass ratio of 4:1:2, grinding the materials uniformly to obtain mixed powder I, spreading the mixed powder I in a ceramic crucible with a cover, then placing the ceramic crucible in a muffle furnace, wherein the initial temperature is 25 ℃, the heating rate is 3 ℃/min, the temperature is increased to 180 ℃, and the mixture is calcined for 2 hours at 180 ℃ to obtain the modified porous polymer.
The slow release reinforcing agent is hydroxymethyl cellulose.
The preparation method of the microbial liquid comprises the following steps:
culturing the thawed Bacillus subtilis, Bacillus megaterium and azotobacter chroococcum by conventional culture method, respectively, and diluting the cultured bacteria liquid to concentration of 1 × 10 8 Obtaining a diluent after cfu/mL, and mixing the bacillus subtilis diluent, the bacillus megaterium diluent and the azotobacter chroococcum diluent according to the mass ratio of 1:3:2 to obtain the microbial solution.
The preparation method of the fixing liquid comprises the following steps:
according to the mass parts, 10 parts of calcium chloride and 30 parts of boric acid are added into 100 parts of water and stirred uniformly to obtain the stationary liquid.
Example 3
A preparation method of a long-acting microbial compound fertilizer comprises the following steps:
according to the mass parts, 40 parts of embedding liquid is taken by an injector with the caliber of 2mm, the embedding liquid is dripped into 100 parts of fixing liquid at the dripping speed of 5mL/min, the fixing liquid is solidified for 2 hours at the rotating speed of 60rpm and then filtered to obtain a solidified substance, and the solidified substance is washed by water for 3 times and then naturally dried at the temperature of 30 ℃ to obtain the long-acting microbial compound fertilizer.
The preparation method of the embedding liquid comprises the following steps:
adding 8 parts by mass of modified porous polymer, 15 parts by mass of sodium alginate and 13 parts by mass of slow-release reinforcing agent into 120 parts by mass of water, stirring at 50 ℃ and 100rpm for 10min, sterilizing at 110 ℃ for 30min, cooling to room temperature, adding 10 parts by mass of microbial solution and 30 parts by mass of potassium dihydrogen phosphate, and continuously stirring at 100rpm for 15min to obtain the embedding solution.
The preparation method of the modified porous polymer comprises the following steps:
t1: adding 2 parts of melamine and 6 parts of p-aldehyde benzoic acid into 50 parts of o-xylene according to parts by mass, condensing and refluxing for 10 hours at 155 ℃, cooling to room temperature, performing suction filtration to obtain a filter cake A, and performing vacuum drying on the filter cake A for 10 hours at 80 ℃ to obtain a ligand;
t2: adding 3 parts by mass of ligand obtained in T1, 3 parts by mass of cobalt nitrate hexahydrate and 2 parts by mass of stannic chloride dihydrate into 50 parts by mass of mixed solution, putting into a reaction kettle, reacting at 120 ℃ for 48 hours, cooling to room temperature, carrying out suction filtration to obtain a filter cake B, and carrying out vacuum drying on the filter cake B at 80 ℃ for 10 hours to obtain a porous polymer, wherein the mixed solution is prepared by mixing N, N-dimethylformamide and ethylenediamine according to a mass ratio of 1: 1;
t3: mixing the porous polymer obtained in the step T2 and Li 2 CO 3 、La 2 O 3 Mixing according to the mass ratio of 4:1:2, grinding uniformly to obtain mixed powder I, flatly paving the mixed powder I in a ceramic crucible with a cover, then placing the ceramic crucible in a muffle furnace, wherein the initial temperature is 25 ℃, the heating rate is 3 ℃/min, and the temperature is raisedCalcining at 180 ℃ for 2 hours to obtain the modified porous polymer.
The slow release reinforcing agent is sodium lignosulphonate.
The preparation method of the microbial liquid comprises the following steps:
culturing the thawed Bacillus subtilis, Bacillus megaterium and azotobacter chroococcum by conventional culture method, respectively, and diluting the cultured bacteria liquid to concentration of 1 × 10 8 Obtaining a diluent after cfu/mL, and mixing the bacillus subtilis diluent, the bacillus megaterium diluent and the azotobacter chroococcum diluent according to the mass ratio of 1:3:2 to obtain the microbial solution.
The preparation method of the fixing liquid comprises the following steps:
according to the mass parts, 10 parts of calcium chloride and 30 parts of boric acid are added into 100 parts of water and stirred uniformly to obtain the stationary liquid.
Example 4
A preparation method of a long-acting microbial compound fertilizer comprises the following steps:
according to the mass parts, 40 parts of embedding liquid is taken by an injector with the caliber of 2mm, the embedding liquid is dripped into 100 parts of fixing liquid at the dripping speed of 5mL/min, the fixing liquid is solidified for 2 hours at the rotating speed of 60rpm and then filtered to obtain a solidified substance, and the solidified substance is washed by water for 3 times and then naturally dried at the temperature of 30 ℃ to obtain the long-acting microbial compound fertilizer.
The preparation method of the embedding liquid comprises the following steps:
adding 8 parts by mass of modified porous polymer, 15 parts by mass of sodium alginate and 13 parts by mass of slow-release reinforcing agent into 120 parts by mass of water, stirring at 50 ℃ and 100rpm for 10min, sterilizing at 110 ℃ for 30min, cooling to room temperature, adding 10 parts by mass of microbial solution and 30 parts by mass of potassium dihydrogen phosphate, and continuously stirring at 100rpm for 15min to obtain the embedding solution.
The preparation method of the modified porous polymer comprises the following steps:
t1: adding 2 parts of melamine and 6 parts of p-aldehyde benzoic acid into 50 parts of o-xylene according to parts by mass, condensing and refluxing for 10 hours at 155 ℃, cooling to room temperature, performing suction filtration to obtain a filter cake A, and performing vacuum drying on the filter cake A for 10 hours at 80 ℃ to obtain a ligand;
t2: adding 3 parts by mass of ligand obtained in T1, 3 parts by mass of cobalt nitrate hexahydrate and 2 parts by mass of stannic chloride dihydrate into 50 parts by mass of mixed solution, putting into a reaction kettle, reacting at 120 ℃ for 48 hours, cooling to room temperature, carrying out suction filtration to obtain a filter cake B, and carrying out vacuum drying on the filter cake B at 80 ℃ for 10 hours to obtain a porous polymer, wherein the mixed solution is prepared by mixing N, N-dimethylformamide and ethylenediamine according to a mass ratio of 1: 1;
t3: mixing the porous polymer obtained in the step T2 and Li 2 CO 3 、La 2 O 3 Mixing the materials according to a mass ratio of 4:1:2, grinding the materials uniformly to obtain 34 mixed powder I, spreading the mixed powder I in a porcelain crucible with a cover, then placing the porcelain crucible in a muffle furnace, wherein the initial temperature is 25 ℃, the heating rate is 3 ℃/min, the temperature is increased to 180 ℃, and the mixture is calcined for 2 hours at 180 ℃ to obtain the modified porous polymer.
The slow release reinforcing agent is formed by mixing hydroxymethyl cellulose and sodium lignin sulfonate according to the mass ratio of 1: 2.
The preparation method of the microbial liquid comprises the following steps: culturing the thawed Bacillus subtilis, Bacillus megaterium and azotobacter chroococcum by conventional culture method, respectively, and diluting the cultured bacteria liquid to concentration of 1 × 10 8 Obtaining a diluent after cfu/mL, and mixing the bacillus subtilis diluent, the bacillus megaterium diluent and the azotobacter chroococcum diluent according to the mass ratio of 1:3:2 to obtain the microbial solution.
The preparation method of the fixing liquid comprises the following steps:
according to the mass parts, 10 parts of calcium chloride and 30 parts of boric acid are added into 100 parts of water and stirred uniformly to obtain the stationary liquid.
Comparative example 1
A preparation method of a long-acting microbial compound fertilizer comprises the following steps:
According to the mass parts, 40 parts of embedding liquid is taken by an injector with the caliber of 2mm, the embedding liquid is dripped into 100 parts of fixing liquid at the dripping speed of 5mL/min, the fixing liquid is solidified for 2 hours at the rotating speed of 100rpm and then filtered to obtain a solidified substance, and the solidified substance is washed by water for 3 times and then naturally dried at the temperature of 30 ℃ to obtain the long-acting microbial compound fertilizer.
The preparation method of the embedding liquid comprises the following steps:
adding 8 parts of porous polymer and 15 parts of sodium alginate into 120 parts of water according to parts by mass, stirring at 50 ℃ and 100rpm for 10min, sterilizing at 110 ℃ for 30min, cooling to room temperature, adding 10 parts of microbial liquid and 30 parts of potassium dihydrogen phosphate, and continuously stirring at 100rpm for 15min to obtain the embedding liquid.
The preparation method of the porous polymer comprises the following steps:
t1: adding 2 parts of melamine and 6 parts of p-aldehyde benzoic acid into 50 parts of o-xylene according to parts by mass, condensing and refluxing for 10 hours at 155 ℃, cooling to room temperature, performing suction filtration to obtain a filter cake A, and performing vacuum drying on the filter cake A for 10 hours at 80 ℃ to obtain a ligand;
t2: adding 3 parts by mass of the ligand obtained in T1, 3 parts by mass of cobalt nitrate hexahydrate and 2 parts by mass of stannic chloride dihydrate into 50 parts by mass of a mixed solution, putting the mixed solution into a reaction kettle, reacting at 120 ℃ for 48 hours, cooling to room temperature, carrying out suction filtration to obtain a filter cake B, and carrying out vacuum drying on the filter cake B at 80 ℃ for 10 hours to obtain a porous polymer, wherein the mixed solution is prepared by mixing N, N-dimethylformamide and ethylenediamine according to a mass ratio of 1: 1.
The preparation method of the microbial liquid comprises the following steps:
culturing the thawed Bacillus subtilis, Bacillus megaterium and azotobacter chroococcum by conventional culture method, respectively, and diluting the cultured bacteria liquid to concentration of 1 × 10 8 Obtaining a diluent after cfu/mL, and mixing the bacillus subtilis diluent, the bacillus megaterium diluent and the azotobacter chroococcum diluent according to the mass ratio of 1:3:2 to obtain the microbial solution.
The preparation method of the fixing liquid comprises the following steps:
according to the mass part, 10 parts of calcium chloride and 30 parts of boric acid are added into 100 parts of water and evenly stirred to obtain the stationary liquid.
Test example 1
The long-acting microbial compound fertilizer prepared in each example and comparative example is subjected to a fertilization effect test, and the fertilizer with the area of 25m is selected from Feixing county of the Compound Fertilizer City 2 The test field with the same land condition is used for planting corn, the plant spacing is 40cm, the mature corn is harvested after three months, and the corn yield is obtained by peeling corn particles and weighing. Applying 1kg of the long-acting microbial compound fertilizer in the embodiment and the comparative example to a test field before planting corn, loosening soil and sowing after three days, then managing according to a traditional corn management mode, and sampling soil by adopting a five-point sampling method for testing effective phosphorus and effective nitrogen in the soil in 1 month, 2 months and 3 months after applying the fertilizer, wherein the testing method comprises the following steps:
And (3) measuring available phosphorus and available potassium of the soil: the soil available phosphorus is measured by adopting a molybdenum-antimony colorimetric-resistance method; the effective potassium in the soil is measured by adopting an ammonium acetate leaching-flame photometry, and the measuring method refers to soil agro-chemical analysis (Boston 2008).
Table 1: soil available phosphorus content table (unit: mg. kg) -1 )
Table 2: soil available potassium content table (unit: mg. kg) -1 )
Table 3: the total mass (unit: kg) of the harvested maize
| Test items | Total mass of corn |
| Example 1 | 17.2 |
| Example 2 | 18.4 |
| Example 3 | 18.5 |
| Example 4 | 18.7 |
| Comparative example 1 | 15.5 |
As can be seen from the data in tables 1, 2 and 3, the modification of the porous polymer in example 1 improves microbial activity, thereby increasing available phosphorus, available potassium and corn yield in soil, compared to comparative example 1; the slow release reinforcing agent hydroxymethyl cellulose is added in the embodiment 2, so that the thickening effect is good, and the agglomeration phenomenon of the modified porous polymer can be reduced; in the embodiment 3, the sustained-release reinforcing agent sodium lignosulfonate is added to form a three-dimensional network space structure on the surface of the modified porous polymer, and the polymerization of the modified porous polymer can be effectively avoided due to electrostatic repulsion; the embodiment 4, the slow release reinforcing agent is the combined action of the hydroxymethyl cellulose and the ammonium lignosulfonate, and the sodium lignosulfonate can reinforce the interaction between the hydroxymethyl cellulose to form an interpenetrating network structure, improve the mechanical stability of the microbial carrier and realize stable slow release.
Test example 2
The slow release effect test of the long-acting microbial compound fertilizer prepared in each embodiment and comparative example comprises the following specific test methods: at 25 ℃, 0.1g of the long-acting microbial compound fertilizer prepared in the example and the comparative example is respectively added into 100mL of deionized water, stirred at the rotating speed of 50rpm, and respectively subjected to 1h, 4h, 8h, 16h, 24h, 48h, 72h, 96h, 120h, 144h and 168h, the release condition of the microbial bacteria in the long-acting microbial compound fertilizer is tested, and the quantity of the microbial bacteria is measured by adopting a dilution plating method.
Table 4: microbial bacteria sustained release (unit: cfu/mL)
| Time (h) | Example 1 | Example 4 | Comparative example 1 |
| 1 | / | / | / |
| 4 | / | / | / |
| 8 | / | / | 2.1×10 3 |
| 16 | 3.4×10 3 | 2.7×10 3 | 8.3×10 3 |
| 24 | 8.5×10 3 | 5.8×10 3 | 1.2×10 4 |
| 48 | 1.4×10 4 | 1.5×10 4 | 2.4×10 4 |
| 72 | 2.6×10 4 | 4.7×10 4 | 3.5×10 4 |
| 96 | 4.5×10 4 | 9.8×10 4 | 4.8×10 4 |
| 120 | 6.8×10 4 | 2.0×10 5 | 6.7×10 4 |
| 144 | 8.4×10 4 | 3.9×10 5 | 7.9×10 4 |
| 168 | 1.7×10 5 | 6.1×10 5 | 9.4×10 4 |
As can be seen from table 4, in the long-acting microbial compound fertilizer prepared in comparative example 1 and example 1, the microbial concentration is released faster in the initial period of slow release and the concentration increase in the later period of slow release tends to be stable after the slow release treatment is performed once, and in the embedding liquid in the long-acting microbial compound fertilizer in example 4, the total microbial concentration is increased slower in the initial period of slow release, and as time goes on, the microbial concentration is increased faster and the microbial concentration increase in the later period is slowed down, but the amount of the microbes is still increased, so that the fertilizer can be utilized more effectively.
Claims (8)
1. The preparation method of the long-acting microbial compound fertilizer is characterized by comprising the following steps of:
and (3) dripping the embedded liquid into the stationary liquid, stirring and solidifying, filtering to obtain a solidified substance, washing the obtained solidified substance with water, and naturally airing to obtain the long-acting microbial compound fertilizer.
2. The method for preparing a long-acting microbial compound fertilizer as claimed in claim 1, comprising the steps of:
according to the mass parts, 40-50 parts of embedding liquid are dripped into 100-120 parts of fixing liquid at the dripping speed of 3-5 mL/min, the fixing liquid is solidified for 1-3 hours at the rotating speed of 60-80 rpm, then the obtained solidified material is filtered to obtain a solidified material, and the solidified material is washed by water and naturally dried at the temperature of 25-35 ℃ to obtain the long-acting microbial compound fertilizer.
3. The method for preparing a long-acting microbial compound fertilizer as claimed in claim 2, wherein the method for preparing the embedding solution comprises the following steps:
according to the mass parts, 8-10 parts of modified porous polymer, 10-15 parts of sodium alginate and 12-14 parts of slow release reinforcing agent are added into 100-120 parts of water, the mixture is stirred at 45-55 ℃ and 100-200 rpm for 10-15 min, then sterilized at 100-110 ℃ for 20-30 min, cooled to room temperature, 10-15 parts of microbial liquid and 30-40 parts of potassium dihydrogen phosphate are added, and the mixture is stirred at 100-200 rpm for 15-25 min to obtain the embedding liquid.
4. The method for preparing a long-acting microbial compound fertilizer as claimed in claim 3, wherein the method for preparing the modified porous polymer comprises the following steps:
t1: adding 1-2 parts by mass of melamine and 4-6 parts by mass of p-aldehyde benzoic acid into 50-60 parts by mass of o-xylene, condensing and refluxing for 8-10 h at 155-165 ℃, cooling to room temperature, performing suction filtration to obtain a filter cake A, and performing vacuum drying on the filter cake A for 8-10 h at 70-80 ℃ to obtain a ligand;
t2: adding 3-5 parts by mass of a ligand obtained in T1, 2-4 parts by mass of cobalt nitrate hexahydrate and 1-3 parts by mass of stannic chloride dihydrate into 50-60 parts by mass of a mixed solution formed by mixing N, N-dimethylformamide and ethylenediamine according to a mass ratio of 1 (1-2), putting the mixed solution into a reaction kettle, reacting for 36-48 h at 120-140 ℃, cooling to room temperature, carrying out suction filtration to obtain a filter cake B, and carrying out vacuum drying on the filter cake B at 70-80 ℃ for 8-10 h to obtain a porous polymer;
t3: mixing the porous polymer obtained in the step T2 and Li 2 CO 3 、La 2 O 3 Mixing the materials according to the mass ratio of (4-6) to (1-3), grinding uniformly to obtain mixed powder I, spreading the mixed powder I in a ceramic crucible with a cover, then placing the ceramic crucible in a muffle furnace, heating to 170-200 ℃ at the initial temperature of 20-25 ℃ at the heating rate of 2-4 ℃/min, and calcining at 170-200 ℃ for 1.5-2.5 hours to obtain the modified porous polymer.
5. The method for preparing a long-acting microbial compound fertilizer as claimed in claim 3, wherein the slow-release enhancer is at least one of hydroxymethyl cellulose, sodium hydroxymethyl cellulose, lignin and sodium lignosulfonate.
6. The method for preparing a long-acting microbial compound fertilizer as claimed in claim 3, wherein the method for preparing the microbial liquid comprises the following steps:
culturing the thawed Bacillus subtilis, Bacillus megaterium and azotobacter chroococcum by conventional culture method, respectively, and diluting the cultured bacteria liquid to the same concentration of 1 × 10 7 ～1×10 8 Obtaining a diluent after cfu/mL, and mixing the bacillus subtilis diluent, the bacillus megaterium diluent and the azotobacter chroococcum diluent according to the mass ratio of 1 (2-4): (1-3) mixing to obtain the microbial liquid.
7. The method for preparing a long-acting microbial compound fertilizer as claimed in claim 2, wherein the method for preparing the fixing solution comprises the following steps: according to the mass parts, 8-12 parts of calcium chloride and 25-30 parts of boric acid are added into 100-120 parts of water and uniformly stirred to obtain the stationary liquid.
8. A long-acting microbial compound fertilizer characterized by being prepared by the method as claimed in any one of claims 1 to 8.
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