CN111440029A - Traditional Chinese medicine residue slow-release fertilizer - Google Patents
Traditional Chinese medicine residue slow-release fertilizer Download PDFInfo
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- CN111440029A CN111440029A CN202010260858.7A CN202010260858A CN111440029A CN 111440029 A CN111440029 A CN 111440029A CN 202010260858 A CN202010260858 A CN 202010260858A CN 111440029 A CN111440029 A CN 111440029A
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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
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Abstract
The invention discloses a traditional Chinese medicine residue slow-release fertilizer which is characterized by comprising 30-40 parts of inorganic components, 35-45 parts of organic components, 10-15 parts of porous cyclodextrin polymers, 0.2-0.5 part of chitosan and 30-40 parts of 1, 3-diglycidyl-5, 5-dimethylhydantoin/1, 4-bis (3-aminopropoxy) butane phosphorus-containing potassium ion type condensation polymers. The invention also discloses a preparation method of the traditional Chinese medicine residue slow-release fertilizer. The traditional Chinese medicine residue slow-release fertilizer disclosed by the invention has the advantages of better slow-release effect, higher fertilizer utilization rate, longer fertilizer efficiency durability, lower cost, safer and more environment-friendly use and capability of effectively realizing good combination of economic benefit, social benefit and ecological benefit.
Description
Technical Field
The invention relates to the technical field of fertilizers, in particular to a traditional Chinese medicine residue slow-release fertilizer and a preparation method thereof.
Background
China is a big agricultural country and a big country for producing and consuming chemical fertilizers, and the total yield and the total consumption of the chemical fertilizers in China are the first in the world. However, agricultural production practices show that the low fertilizer utilization rate is a common problem in the fertilizer use process due to the comprehensive influence of the fertilizer properties and the soil environment conditions. Especially in recent years, blind application of inorganic chemical fertilizers leads to reduction of organic matter content in soil, destruction of soil structure, and deterioration of soil nutrient coordination supply capacity, physicochemical properties and biological properties, which leads to deterioration of agricultural product quality, serious environmental pollution and influence on human health.
The fertilizer in the prior art mainly comprises inorganic fertilizer and organic fertilizer. The inorganic fertilizer has strong effect, the application amount is not easy to master, the seedlings are easy to burn, and the soil structure is influenced; the organic fertilizer is not specially treated and is easy to deteriorate to cause small environmental pollution; it is in this situation that slow release fertilizers are produced at the same time. The slow release fertilizer has stable fertilizer efficiency and little pollution to the environment, is basically synchronous with the nutrient absorption of crops by regulating and controlling the nutrient release rate, can greatly improve the nutrient utilization rate of the fertilizer, reduces the agricultural non-point source pollution, and meets the requirements of the national sustainable development strategy, so the slow release fertilizer becomes one of the main directions of the development of the fertilizer industry in the 21 st century.
The existing slow release fertilizer is prepared by coating the active ingredients to achieve slow release, and the coating layer has complex ingredients and certain destructive power after being applied to soil; the preparation method has the disadvantages of complex production process, high manufacturing cost and limited slow release effect, and cannot be popularized and applied in a large area.
The Chinese patent application publication with publication number CN103159530A discloses a slow-release compound fertilizer special for hot pepper and a preparation method thereof, the compound fertilizer comprises a nitrogen fertilizer, a phosphate fertilizer, a potash fertilizer and trace elements of calcium and magnesium boron, and the potash fertilizer is potassium sulfate; the nitrogen fertilizer is urea formaldehyde; the weight portion ratio of the nitrogenous fertilizer, the phosphate fertilizer, the potash fertilizer and the trace elements of calcium, magnesium and boron is N: P2O5:K2Ca, Mg, B-13-15: 8-10:16-18:1.5-2:1.5-2: 0.05-0.1. The method improves the utilization rate of the fertilizer, but the production process involves the reaction of urea and formaldehyde, potassium chloride and sulfuric acid, and the energy consumption is too large.
The production of traditional Chinese medicine is important in the pharmaceutical industry of China, and most of traditional Chinese medicines belong to plant medicines, so the production of traditional Chinese medicines generally adopts solvents to extract active ingredients, and then the dregs of a decoction are not used. A large amount of traditional Chinese medicine dregs are treated by traditional treatment methods such as incineration, landfill or stacking, which causes resource waste and environmental pollution. The waste residue of the traditional Chinese medicine is prepared into the fertilizer, so that the waste resource of the traditional Chinese medicine can be fully utilized, and the waste is changed into valuable.
Therefore, the traditional Chinese medicine residue slow-release fertilizer which has the advantages of better slow-release effect, higher fertilizer utilization rate, longer fertilizer effect durability, lower cost and safer and more environment-friendly use is developed, meets the market demand, has very large market value and application prospect, and has very important significance for promoting the development of the slow-release fertilizer industry.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides the traditional Chinese medicine residue slow-release fertilizer and the preparation method thereof, and the preparation method has the advantages of simple and feasible process, low cost, environment-friendly raw materials, low investment and high production efficiency, and is suitable for continuous large-scale production; the traditional Chinese medicine residue slow-release fertilizer prepared by the preparation method has the advantages of better slow-release effect, higher fertilizer utilization rate, longer fertilizer efficiency durability, lower cost, safer and more environment-friendly use and capability of effectively realizing good combination of economic benefit, social benefit and ecological benefit.
In order to achieve the purpose of the invention, the technical scheme adopted by the invention is as follows: the traditional Chinese medicine residue slow-release fertilizer is characterized by comprising 30-40 parts of inorganic components, 35-45 parts of organic components, 10-15 parts of porous cyclodextrin polymers, 0.2-0.5 part of chitosan and 30-40 parts of 1, 3-diglycidyl-5, 5-dimethylhydantoin/1, 4-bis (3-aminopropoxy) butane phosphorus-containing potassium ion-type polycondensate.
Preferably, the inorganic component comprises the following components in parts by weight: 1-3 parts of calcium peroxide, 15-25 parts of potassium nitrate, 10-15 parts of phosphorus pentoxide and 20-30 parts of urea particles.
Preferably, the organic component comprises the following components in parts by weight: 3-6 parts of traditional Chinese medicine residues, 10-15 parts of dry cow dung, 10-15 parts of wood dust powder and 8-10 parts of sunflower meal.
Preferably, the preparation method of the organic component comprises the following steps: uniformly mixing the components in parts by weight to obtain a mixture, performing compost fermentation for three days, turning the compost 1-3 times every day, keeping the fermentation for 9-15 days, and screening and crushing the fermentation product to obtain the organic component.
Preferably, the herb residue comprises at least one of mint, angelica dahurica, astragalus mongholicus, dried orange peel and salvia miltiorrhiza.
Preferably, the preparation method of the porous cyclodextrin polymer is as follows: chinese patent application No. 201510674629.9, example 1.
Preferably, the chitosan has a weight average molecular weight of 10 ten thousand and a degree of deacetylation of 95%.
Preferably, the preparation method of the 1, 3-diglycidyl-5, 5-dimethylhydantoin/1, 4-bis (3-aminopropoxy) butane phosphorus-containing potassium ion-type polycondensate comprises the following steps:
step S1, adding 1, 3-diglycidyl-5, 5-dimethylhydantoin, 1, 4-bis (3-aminopropoxy) butane and an alkaline catalyst into a high-boiling-point solvent, stirring and reacting for 4-6 hours at 75-85 ℃, filtering to remove insoluble substances, and performing rotary evaporation to remove the solvent to obtain a polycondensate;
step S2, dissolving the polycondensate prepared in the step S1 in N-methyl pyrrolidone, adding chloromethyl phosphoric acid into the polycondensate, stirring the mixture for 6 to 8 hours at the temperature of between 60 and 80 ℃, and then removing the N-methyl pyrrolidone through rotary evaporation to obtain an ionized polycondensate;
and S3, dissolving the ionized polycondensate prepared in the S2 in water, adding potassium hydroxide into the water, adjusting the pH to 6.5-7.5, and then performing rotary evaporation to remove the water to obtain the phosphorus-potassium-containing 1, 3-diglycidyl-5, 5-dimethylhydantoin/1, 4-bis (3-aminopropoxy) butane ionic polycondensate.
Preferably, the molar ratio of the 1, 3-diglycidyl-5, 5-dimethylhydantoin, the 1, 4-bis (3-aminopropoxy) butane, the basic catalyst and the high-boiling point solvent in the step S1 is 1:1 (0.8-1.2) to (6-10).
Preferably, the alkaline catalyst is at least one of potassium hydroxide, sodium carbonate, potassium carbonate and sodium hydroxide; the high boiling point solvent is at least one of dimethyl sulfoxide, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone.
Preferably, the mass ratio of the polycondensate, the N-methylpyrrolidone and the chloromethyl phosphoric acid in the step S2 is 1 (5-10) to (0.2-0.4).
Preferably, the mass ratio of the ionized polycondensate to the water in step S3 is 1 (3-5).
Another object of the present invention is to provide a preparation method of the slow release fertilizer containing traditional Chinese medicine residues, which is characterized by comprising the following steps: uniformly mixing an inorganic component, an organic component, a porous cyclodextrin polymer and chitosan, and grinding into powder; and then crosslinking the obtained powder by using 1, 3-diglycidyl-5, 5-dimethylhydantoin/1, 4-bis (3-aminopropoxy) butane phosphorus-containing potassium ion polycondensate, and extruding the crosslinked powder into fertilizer particles to obtain the traditional Chinese medicine residue slow release fertilizer.
Adopt the produced beneficial effect of above-mentioned technical scheme to lie in:
(1) the preparation method of the traditional Chinese medicine residue slow-release fertilizer provided by the invention has the advantages of simple and feasible process, low cost, environment-friendly raw materials, low investment and high production efficiency, and is suitable for continuous large-scale production.
(2) The traditional Chinese medicine residue slow-release fertilizer overcomes the defects that the traditional inorganic fertilizer has strong fertilizer effect, is not easy to master application amount, is easy to burn seedlings and influences the soil structure; the organic fertilizer is not specially treated and is easy to deteriorate to cause small environmental pollution, and the defects that the active ingredients are coated to achieve slow release in the conventional slow release fertilizer, and the coating layer has complex components and certain destructive power after being applied to soil are overcome; the slow-release fertilizer has the technical problems of complex production process, high manufacturing cost, limited slow-release effect and incapability of being popularized and applied in a large area, and has the advantages of better slow-release effect, higher fertilizer utilization rate, longer fertilizer efficiency durability, lower cost, safer and more environment-friendly use and capability of effectively realizing good combination of economic benefit, social benefit and ecological benefit.
(3) The traditional Chinese medicine residue slow release fertilizer provided by the invention takes 1, 3-diglycidyl-5, 5-dimethylhydantoin/1, 4-bis (3-aminopropoxy) butane phosphorus-potassium-containing ionic polycondensate as a coating adhesive body, and can improve the slow release effect of nutrients through two modes of physical adsorption and chemical bonding, thereby realizing the improvement of the utilization rate of the fertilizer; the degradable organic fertilizer has degradable performance, and the degraded product can supplement nutrients such as nitrogen, phosphorus, potassium and the like, increase the content of organic matters in soil, improve the physical and chemical properties of low-yield soil and contribute to the growth of microbial communities in the soil; the amphoteric salt structure is beneficial to improving the slow release effect, regulating the PH and promoting the growth of crops; and it has the functions of eliminating harmful microbe, reducing crop morbidity and promoting crop growth.
(4) According to the traditional Chinese medicine residue slow-release fertilizer provided by the invention, the porous cyclodextrin polymer is added, organic components and inorganic components can enter the porous structure and the cavity structure of cyclodextrin, and when the fertilizer is applied, the fertilizer is slowly released and discharged from the porous structure and the cavity structure of cyclodextrin, so that the slow-release effect is realized, the fertilizer efficiency is enhanced, and the loss and waste are reduced. The organic phosphorus pesticide residue in the soil can be adsorbed, and the soil can be purified and restored; the chitosan-chitosan composite has synergistic effect with chitosan, has controlled release effect, and is beneficial to promoting rooting and plant growth; the fertilizer nutrient molecules are absorbed under the action of hydrogen bonds, surface tension, van der waals force and viscous force, and the migration rate of fertilizer nutrients along with water flow is slowed down, so that the fertilizer nutrient loss is controlled.
(5) According to the traditional Chinese medicine residue slow-release fertilizer provided by the invention, the inorganic component contains calcium peroxide, and calcium hydroxide and oxygen which can improve acid soil can be generated easily by reaction when water is added, so that the indoor oxygen content can be increased; the traditional Chinese medicine residues are added into the organic components, so that waste is changed into valuable, energy is saved, and the environment is protected; the components have synergistic effect, so that the fertilizer efficiency is better and the slow release effect is better.
Detailed Description
In order to make the technical solutions of the present invention better understood and make the above features, objects, and advantages of the present invention more comprehensible, the present invention is further described with reference to the following examples. The examples are intended to illustrate the invention only and are not intended to limit the scope of the invention.
The preparation of the porous cyclodextrin polymers referred to in the following examples of the invention is described in: chinese invention patent example 1 with application number 201510674629.9; the weight average molecular weight of the chitosan is 10 ten thousand, and the deacetylation degree is 95%; other raw materials were all purchased commercially.
Example 1
The traditional Chinese medicine residue slow-release fertilizer is characterized by comprising 30 parts of inorganic components, 35 parts of organic components, 10 parts of porous cyclodextrin polymers, 0.2 part of chitosan and 30 parts of 1, 3-diglycidyl-5, 5-dimethylhydantoin/1, 4-bis (3-aminopropoxy) butane phosphorus-containing potassium ion type condensation polymers.
The inorganic component comprises the following components in parts by weight: 1 part of calcium peroxide, 15 parts of potassium nitrate, 10 parts of phosphorus pentoxide and 20 parts of urea particles.
The organic component comprises the following components in parts by weight: 3 parts of traditional Chinese medicine residues, 10 parts of dry cow dung, 10 parts of wood chip powder and 8 parts of sunflower meal.
The preparation method of the organic component comprises the following steps: uniformly mixing the components in parts by weight to obtain a mixture, performing compost fermentation, turning the compost for 1 time every day after three days of compost fermentation, keeping the fermentation for 9 days all the time, and screening and crushing the fermentation product to obtain an organic component; the traditional Chinese medicine residues comprise a mixture obtained by mixing mint, angelica dahurica, astragalus mongholicus, dried orange peel and salvia miltiorrhiza according to a mass ratio of 1:2:3:2: 2.
The preparation method of the 1, 3-diglycidyl-5, 5-dimethylhydantoin/1, 4-bis (3-aminopropoxy) butane phosphorus-containing potassium ion polycondensate comprises the following steps:
step S1, adding 1, 3-diglycidyl-5, 5-dimethylhydantoin, 1, 4-bis (3-aminopropoxy) butane and potassium hydroxide into dimethyl sulfoxide, stirring and reacting for 4 hours at 75 ℃, filtering to remove insoluble substances, and performing rotary evaporation to remove the solvent to obtain a polycondensate; the molar ratio of the 1, 3-diglycidyl-5, 5-dimethylhydantoin to the 1, 4-bis (3-aminopropoxy) butane to the potassium hydroxide to the dimethyl sulfoxide is 1:1:0.8: 6;
step S2, dissolving the polycondensate prepared in the step S1 in N-methyl pyrrolidone, adding chloromethyl phosphoric acid into the polycondensate, stirring the mixture at the temperature of 60 ℃ for 6 hours, and performing rotary evaporation to remove the N-methyl pyrrolidone to obtain an ionized polycondensate; the mass ratio of the polycondensate to the N-methylpyrrolidone to the chloromethyl phosphoric acid is 1:5: 0.2;
step S3, dissolving the ionized polycondensate prepared in the step S2 in water, adding potassium hydroxide into the water, adjusting the pH to 6.5, and then removing water by rotary evaporation to obtain 1, 3-diglycidyl-5, 5-dimethylhydantoin/1, 4-bis (3-aminopropoxy) butane phosphorus-potassium-containing ionic polycondensate; the mass ratio of the ionized polycondensate to the water is 1:3.
The preparation method of the traditional Chinese medicine residue slow-release fertilizer is characterized by comprising the following steps of: uniformly mixing an inorganic component, an organic component, a porous cyclodextrin polymer and chitosan, and grinding into powder; and then crosslinking the obtained powder by using 1, 3-diglycidyl-5, 5-dimethylhydantoin/1, 4-bis (3-aminopropoxy) butane phosphorus-containing potassium ion polycondensate, and extruding the crosslinked powder into fertilizer particles to obtain the traditional Chinese medicine residue slow release fertilizer.
Example 2
The traditional Chinese medicine residue slow-release fertilizer is characterized by comprising 33 parts of inorganic components, 38 parts of organic components, 12 parts of porous cyclodextrin polymers, 0.3 part of chitosan and 32 parts of 1, 3-diglycidyl-5, 5-dimethylhydantoin/1, 4-bis (3-aminopropoxy) butane phosphorus-potassium-containing ionic polycondensate.
The inorganic component comprises the following components in parts by weight: 1.5 parts of calcium peroxide, 17 parts of potassium nitrate, 11 parts of phosphorus pentoxide and 22 parts of urea particles.
The organic component comprises the following components in parts by weight: 4 parts of traditional Chinese medicine residues, 11 parts of dried cow dung, 12 parts of wood chip powder and 8.5 parts of sunflower meal.
The preparation method of the organic component comprises the following steps: uniformly mixing the components in parts by weight to obtain a mixture, performing compost fermentation for three days, turning the compost 2 times every day, keeping the fermentation for 11 days, and screening and crushing the fermentation product to obtain an organic component; the traditional Chinese medicine residues comprise a mixture formed by mixing mint, angelica dahurica, astragalus mongholicus, dried orange peel and salvia miltiorrhiza according to a mass ratio of 1:3:2:3: 2.
The preparation method of the 1, 3-diglycidyl-5, 5-dimethylhydantoin/1, 4-bis (3-aminopropoxy) butane phosphorus-containing potassium ion polycondensate comprises the following steps:
step S1, adding 1, 3-diglycidyl-5, 5-dimethylhydantoin, 1, 4-bis (3-aminopropoxy) butane and sodium carbonate into N, N-dimethylformamide, stirring and reacting for 4.5 hours at 77 ℃, filtering to remove insoluble substances, and performing rotary evaporation to remove the solvent to obtain a polycondensate; the molar ratio of the 1, 3-diglycidyl-5, 5-dimethylhydantoin to the 1, 4-bis (3-aminopropoxy) butane to the sodium carbonate to the N, N-dimethylformamide is 1:1:0.9: 7;
step S2, dissolving the polycondensate prepared in the step S1 in N-methyl pyrrolidone, adding chloromethyl phosphoric acid into the polycondensate, stirring the mixture at 65 ℃ for 6.5 hours, and performing rotary evaporation to remove the N-methyl pyrrolidone to obtain an ionized polycondensate; the mass ratio of the polycondensate to the N-methylpyrrolidone to the chloromethyl phosphoric acid is 1:6: 0.25;
step S3, dissolving the ionized polycondensate prepared in the step S2 in water, adding potassium hydroxide into the water, adjusting the pH to 6.8, and then removing water by rotary evaporation to obtain 1, 3-diglycidyl-5, 5-dimethylhydantoin/1, 4-bis (3-aminopropoxy) butane phosphorus-potassium-containing ionic polycondensate; the mass ratio of the ionized polycondensate to the water is 1: 3.5.
The preparation method of the traditional Chinese medicine residue slow-release fertilizer is characterized by comprising the following steps of: uniformly mixing an inorganic component, an organic component, a porous cyclodextrin polymer and chitosan, and grinding into powder; and then crosslinking the obtained powder by using 1, 3-diglycidyl-5, 5-dimethylhydantoin/1, 4-bis (3-aminopropoxy) butane phosphorus-containing potassium ion polycondensate, and extruding the crosslinked powder into fertilizer particles to obtain the traditional Chinese medicine residue slow release fertilizer.
Example 3
The traditional Chinese medicine residue slow-release fertilizer is characterized by comprising 35 parts of inorganic components, 40 parts of organic components, 13 parts of porous cyclodextrin polymers, 0.35 part of chitosan and 35 parts of 1, 3-diglycidyl-5, 5-dimethylhydantoin/1, 4-bis (3-aminopropoxy) butane phosphorus-potassium-containing ionic polycondensate.
The inorganic component comprises the following components in parts by weight: 2 parts of calcium peroxide, 20 parts of potassium nitrate, 13 parts of phosphorus pentoxide and 25 parts of urea particles.
The organic component comprises the following components in parts by weight: 4.5 parts of traditional Chinese medicine residues, 13 parts of dried cow dung, 13 parts of wood dust powder and 9 parts of sunflower meal.
The preparation method of the organic component comprises the following steps: uniformly mixing the components in parts by weight to obtain a mixture, performing compost fermentation, turning over the compost for 2 times every day after three days of compost fermentation, keeping the fermentation for 12 days all the time, and screening and crushing the fermentation product to obtain an organic component; the traditional Chinese medicine residues comprise a mixture formed by mixing mint, angelica dahurica, astragalus mongholicus and dried orange peel according to a mass ratio of 1:3:2: 1.
The preparation method of the 1, 3-diglycidyl-5, 5-dimethylhydantoin/1, 4-bis (3-aminopropoxy) butane phosphorus-containing potassium ion polycondensate comprises the following steps:
step S1, adding 1, 3-diglycidyl-5, 5-dimethylhydantoin, 1, 4-bis (3-aminopropoxy) butane and potassium carbonate into N, N-dimethylacetamide, stirring and reacting at 80 ℃ for 5 hours, filtering to remove insoluble substances, and performing rotary evaporation to remove the solvent to obtain a polycondensate; the molar ratio of the 1, 3-diglycidyl-5, 5-dimethylhydantoin, the 1, 4-bis (3-aminopropoxy) butane, the potassium carbonate and the N, N-dimethylacetamide is 1:1:1: 8;
step S2, dissolving the polycondensate prepared in the step S1 in N-methyl pyrrolidone, adding chloromethyl phosphoric acid into the polycondensate, stirring the mixture at 70 ℃ for 7 hours, and performing rotary evaporation to remove the N-methyl pyrrolidone to obtain an ionized polycondensate; the mass ratio of the polycondensate to the N-methyl pyrrolidone to the chloromethyl phosphoric acid is 1:8: 0.3;
step S3, dissolving the ionized polycondensate prepared in the step S2 in water, adding potassium hydroxide into the water, adjusting the pH to 7, and then performing rotary evaporation to remove the water to obtain the phosphorus and potassium containing ionic polycondensate of 1, 3-diglycidyl-5, 5-dimethylhydantoin/1, 4-bis (3-aminopropoxy) butane; the mass ratio of the ionized polycondensate to the water is 1:4.
The preparation method of the traditional Chinese medicine residue slow-release fertilizer is characterized by comprising the following steps of: uniformly mixing an inorganic component, an organic component, a porous cyclodextrin polymer and chitosan, and grinding into powder; and then crosslinking the obtained powder by using 1, 3-diglycidyl-5, 5-dimethylhydantoin/1, 4-bis (3-aminopropoxy) butane phosphorus-containing potassium ion polycondensate, and extruding the crosslinked powder into fertilizer particles to obtain the traditional Chinese medicine residue slow release fertilizer.
Example 4
The traditional Chinese medicine residue slow-release fertilizer is characterized by comprising 38 parts of an inorganic component, 44 parts of an organic component, 14 parts of a porous cyclodextrin polymer, 0.45 part of chitosan, and 38 parts of 1, 3-diglycidyl-5, 5-dimethylhydantoin/1, 4-bis (3-aminopropoxy) butane phosphorus-potassium-containing ionic polycondensate.
The inorganic component comprises the following components in parts by weight: 2.5 parts of calcium peroxide, 23 parts of potassium nitrate, 14 parts of phosphorus pentoxide and 28 parts of urea particles.
The organic component comprises the following components in parts by weight: 5 parts of traditional Chinese medicine residues, 14 parts of dried cow dung, 14 parts of wood chip powder and 9.5 parts of sunflower meal.
The preparation method of the organic component comprises the following steps: uniformly mixing the components in parts by weight to obtain a mixture, performing compost fermentation, turning over the compost for 3 times every day after three days of compost fermentation, keeping the fermentation for 13 days all the time, and screening and crushing the fermentation product to obtain an organic component; the traditional Chinese medicine residues comprise a mixture formed by mixing mint and radix angelicae in a mass ratio of 2: 3.
The preparation method of the 1, 3-diglycidyl-5, 5-dimethylhydantoin/1, 4-bis (3-aminopropoxy) butane phosphorus-containing potassium ion polycondensate comprises the following steps:
step S1, adding 1, 3-diglycidyl-5, 5-dimethylhydantoin, 1, 4-bis (3-aminopropoxy) butane and an alkaline catalyst into a high-boiling-point solvent, stirring and reacting for 5.5 hours at 83 ℃, filtering to remove insoluble substances, and performing rotary evaporation to remove the solvent to obtain a polycondensate; the molar ratio of the 1, 3-diglycidyl-5, 5-dimethylhydantoin, the 1, 4-bis (3-aminopropoxy) butane, the basic catalyst and the high-boiling-point solvent is 1:1:1.1: 9; the alkaline catalyst is prepared by mixing potassium hydroxide, sodium carbonate, potassium carbonate and sodium hydroxide according to the mass ratio of 1:2:4: 3; the high-boiling-point solvent is formed by mixing dimethyl sulfoxide, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone according to a mass ratio of 2:1:2: 3;
step S2, dissolving the polycondensate prepared in the step S1 in N-methyl pyrrolidone, adding chloromethyl phosphoric acid into the polycondensate, stirring the mixture at 75 ℃ for 7.5 hours, and performing rotary evaporation to remove the N-methyl pyrrolidone to obtain an ionized polycondensate; the mass ratio of the polycondensate to the N-methylpyrrolidone to the chloromethyl phosphoric acid is 1:9: 0.35;
step S3, dissolving the ionized polycondensate prepared in the step S2 in water, adding potassium hydroxide into the water, adjusting the pH to 7.3, and then removing water by rotary evaporation to obtain 1, 3-diglycidyl-5, 5-dimethylhydantoin/1, 4-bis (3-aminopropoxy) butane phosphorus-potassium-containing ionic polycondensate; the mass ratio of the ionized polycondensate to the water is 1: 4.5.
The preparation method of the traditional Chinese medicine residue slow-release fertilizer is characterized by comprising the following steps of: uniformly mixing an inorganic component, an organic component, a porous cyclodextrin polymer and chitosan, and grinding into powder; and then crosslinking the obtained powder by using 1, 3-diglycidyl-5, 5-dimethylhydantoin/1, 4-bis (3-aminopropoxy) butane phosphorus-containing potassium ion polycondensate, and extruding the crosslinked powder into fertilizer particles to obtain the traditional Chinese medicine residue slow release fertilizer.
Example 5
The traditional Chinese medicine residue slow-release fertilizer is characterized by comprising 40 parts of inorganic components, 45 parts of organic components, 15 parts of porous cyclodextrin polymers, 0.5 part of chitosan and 40 parts of 1, 3-diglycidyl-5, 5-dimethylhydantoin/1, 4-bis (3-aminopropoxy) butane phosphorus-potassium-containing ionic polycondensate.
The inorganic component comprises the following components in parts by weight: 3 parts of calcium peroxide, 25 parts of potassium nitrate, 15 parts of phosphorus pentoxide and 30 parts of urea particles.
The organic component comprises the following components in parts by weight: 6 parts of traditional Chinese medicine residues, 15 parts of dry cow dung, 15 parts of wood chip powder and 10 parts of sunflower meal.
The preparation method of the organic component comprises the following steps: uniformly mixing the components in parts by weight to obtain a mixture, performing compost fermentation, turning over the compost for 3 times every day after three days of compost fermentation, keeping the fermentation for 15 days all the time, and screening and crushing the fermentation product to obtain an organic component; the traditional Chinese medicine residues comprise a mixture formed by mixing mint, astragalus and salvia miltiorrhiza according to the mass ratio of 1:3: 2.
The preparation method of the 1, 3-diglycidyl-5, 5-dimethylhydantoin/1, 4-bis (3-aminopropoxy) butane phosphorus-containing potassium ion polycondensate comprises the following steps:
step S1, adding 1, 3-diglycidyl-5, 5-dimethylhydantoin, 1, 4-bis (3-aminopropoxy) butane and sodium hydroxide into N-methylpyrrolidone, stirring and reacting at 85 ℃ for 6 hours, filtering to remove insoluble substances, and performing rotary evaporation to remove the solvent to obtain a polycondensate; the molar ratio of the 1, 3-diglycidyl-5, 5-dimethylhydantoin to the 1, 4-bis (3-aminopropoxy) butane to the sodium hydroxide to the N-methylpyrrolidone is 1:1:1.2: 10;
step S2, dissolving the polycondensate prepared in the step S1 in N-methyl pyrrolidone, adding chloromethyl phosphoric acid into the polycondensate, stirring the mixture at 80 ℃ for 8 hours, and then performing rotary evaporation to remove the N-methyl pyrrolidone to obtain an ionized polycondensate; the mass ratio of the polycondensate to the N-methyl pyrrolidone to the chloromethyl phosphoric acid is 1:10: 0.4;
step S3, dissolving the ionized polycondensate prepared in the step S2 in water, adding potassium hydroxide into the water, adjusting the pH to 7.5, and then removing water by rotary evaporation to obtain 1, 3-diglycidyl-5, 5-dimethylhydantoin/1, 4-bis (3-aminopropoxy) butane phosphorus-potassium-containing ionic polycondensate; the mass ratio of the ionized polycondensate to the water is 1: 5.
The preparation method of the traditional Chinese medicine residue slow-release fertilizer is characterized by comprising the following steps of: uniformly mixing an inorganic component, an organic component, a porous cyclodextrin polymer and chitosan, and grinding into powder; and then crosslinking the obtained powder by using 1, 3-diglycidyl-5, 5-dimethylhydantoin/1, 4-bis (3-aminopropoxy) butane phosphorus-containing potassium ion polycondensate, and extruding the crosslinked powder into fertilizer particles to obtain the traditional Chinese medicine residue slow release fertilizer.
Comparative example 1
A slow release fertilizer containing herb residue has the same formula and preparation method as those of example 1, except that no calcium peroxide is added.
Comparative example 2
A slow release fertilizer containing herb residue has the same formula and preparation method as those of example 1, except that no herb residue is added.
Comparative example 3
A slow release fertilizer containing herb residue has substantially the same formulation and preparation method as those of example 1, except that no porous cyclodextrin polymer is added.
Comparative example 4
A controlled release fertilizer containing herb residue, formulation and preparation method are substantially the same as example 1, except that 1, 3-diglycidyl-5, 5-dimethylhydantoin/1, 4-bis (3-aminopropoxy) butane polycondensate is used instead of 1, 3-diglycidyl-5, 5-dimethylhydantoin/1, 4-bis (3-aminopropoxy) butane phosphorus-containing potassium ion polycondensate.
Comparative example 5
The commercial pure dry chicken manure organic fertilizer is purchased from Shijiazhuang Fengdi Fei Co.
In order to further illustrate the beneficial technical effects of the embodiment of the invention, the performance test of the traditional Chinese medicine residue slow-release fertilizer of each of the embodiments 1-5 and the comparative examples 1-5 of the invention is respectively carried out, and the test results are shown in table 1; the test method is as follows: applying fertilizer to the roses in the same growth environment, wherein the fertilizer application amount is 10 kg/mu, performing hole application at one time, observing the growth condition of the roses and the peanuts in the same period after the roses reach the flowering phase, and testing the soil quality; the product yield was increased relative to the product of comparative example 5.
Table 1 results of performance test of the slow release fertilizer containing dregs of decoction in examples and comparative examples
| Item | Disease and insect Rate (%) | Product yield (%) | Soil active organic matter (g/kg) |
| Example 1 | 0.3 | 88 | 8.53 |
| Example 2 | 0.2 | 91 | 8.57 |
| Example 3 | 0.2 | 93 | 8.62 |
| Example 4 | 0.1 | 95 | 8.69 |
| Example 5 | 0 | 99 | 8.75 |
| Comparative example 1 | 1.2 | 54 | 8.50 |
| Comparative example 2 | 1.0 | 60 | 6.87 |
| Comparative example 3 | 0.6 | 51 | 7.23 |
| Comparative example 4 | 0.9 | 68 | 8.23 |
| Comparative example 5 | 3.5 | — | 7.35 |
As can be seen from the table above, the disease and insect rate of the traditional Chinese medicine residue slow-release fertilizer disclosed by the invention is 0% -0.3%, the yield of the product is increased by 88% -99% compared with the comparative example, and the active organic matter in the soil is 8.53-8.75 g/kg; the pest and disease rate of the common fertilizer sold in the market is 3.5 percent, and the active organic matter of the soil is 7.35 g/kg; therefore, the traditional Chinese medicine residue slow-release fertilizer disclosed by the invention has stronger pest resistance and more obvious effects on flower yield increase and soil improvement.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are merely illustrative of the principles of the invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. The traditional Chinese medicine residue slow-release fertilizer is characterized by comprising 30-40 parts of inorganic components, 35-45 parts of organic components, 10-15 parts of porous cyclodextrin polymers, 0.2-0.5 part of chitosan and 30-40 parts of 1, 3-diglycidyl-5, 5-dimethylhydantoin/1, 4-bis (3-aminopropoxy) butane phosphorus-containing potassium ion-type polycondensate.
2. The traditional Chinese medicine residue slow-release fertilizer as claimed in claim 1, wherein the inorganic component comprises the following components in parts by weight: 1-3 parts of calcium peroxide, 15-25 parts of potassium nitrate, 10-15 parts of phosphorus pentoxide and 20-30 parts of urea particles.
3. The traditional Chinese medicine residue slow-release fertilizer as claimed in claim 1, wherein the organic component comprises the following components in parts by weight: 3-6 parts of traditional Chinese medicine residues, 10-15 parts of dry cow dung, 10-15 parts of wood dust powder and 8-10 parts of sunflower meal.
4. The traditional Chinese medicine residue slow-release fertilizer as claimed in claim 3, wherein the preparation method of the organic component comprises the following steps: uniformly mixing the components in parts by weight to obtain a mixture, performing compost fermentation for three days, turning the compost 1-3 times every day, keeping the fermentation for 9-15 days, and screening and crushing the fermentation product to obtain the organic component.
5. The slow release fertilizer for traditional Chinese medicine residues as claimed in claim 3, wherein the traditional Chinese medicine residues comprise at least one of mint, angelica dahurica, astragalus mongholicus, dried orange peel and salvia miltiorrhiza.
6. The traditional Chinese medicine dreg slow-release fertilizer as claimed in claim 1, wherein the preparation method of the 1, 3-diglycidyl-5, 5-dimethylhydantoin/1, 4-bis (3-aminopropoxy) butane phosphorus-containing potassium ion-type polycondensate comprises the following steps:
step S1, adding 1, 3-diglycidyl-5, 5-dimethylhydantoin, 1, 4-bis (3-aminopropoxy) butane and an alkaline catalyst into a high-boiling-point solvent, stirring and reacting for 4-6 hours at 75-85 ℃, filtering to remove insoluble substances, and performing rotary evaporation to remove the solvent to obtain a polycondensate;
step S2, dissolving the polycondensate prepared in the step S1 in N-methyl pyrrolidone, adding chloromethyl phosphoric acid into the polycondensate, stirring the mixture for 6 to 8 hours at the temperature of between 60 and 80 ℃, and then removing the N-methyl pyrrolidone through rotary evaporation to obtain an ionized polycondensate;
and S3, dissolving the ionized polycondensate prepared in the S2 in water, adding potassium hydroxide into the water, adjusting the pH to 6.5-7.5, and then performing rotary evaporation to remove the water to obtain the phosphorus-potassium-containing 1, 3-diglycidyl-5, 5-dimethylhydantoin/1, 4-bis (3-aminopropoxy) butane ionic polycondensate.
7. The slow-release fertilizer containing herb residue of claim 6, wherein the molar ratio of 1, 3-diglycidyl-5, 5-dimethylhydantoin, 1, 4-bis (3-aminopropoxy) butane, the basic catalyst and the high-boiling point solvent in step S1 is 1:1 (0.8-1.2) to (6-10).
8. The traditional Chinese medicine residue slow-release fertilizer as claimed in claim 6, wherein the alkaline catalyst is at least one of potassium hydroxide, sodium carbonate, potassium carbonate and sodium hydroxide; the high boiling point solvent is at least one of dimethyl sulfoxide, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone.
9. The traditional Chinese medicine residue slow-release fertilizer as claimed in claim 6, wherein the mass ratio of the polycondensate, the N-methyl pyrrolidone and the chloromethyl phosphoric acid in the step S2 is 1 (5-10) to (0.2-0.4); the mass ratio of the ionized polycondensate to the water in step S3 is 1 (3-5).
10. The traditional Chinese medicine residue slow-release fertilizer as claimed in any one of claims 1 to 9, wherein the preparation method of the traditional Chinese medicine residue slow-release fertilizer comprises the following steps: uniformly mixing an inorganic component, an organic component, a porous cyclodextrin polymer and chitosan, and grinding into powder; and then crosslinking the obtained powder by using 1, 3-diglycidyl-5, 5-dimethylhydantoin/1, 4-bis (3-aminopropoxy) butane phosphorus-containing potassium ion polycondensate, and extruding the crosslinked powder into fertilizer particles to obtain the traditional Chinese medicine residue slow release fertilizer.
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