A fertilizer synergist and method of making same
By combining sludge from wastewater treatment plants and rice bran extract with other components, a fertilizer synergist was developed, which solved the problems of low nitrogen fertilizer utilization and short-lived fertilizer effect, achieving stable and efficient nutrient supply and environmental benefits.
Patent Information
- Application Number
- CN202510358534.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-03-25
- Publication Date
- 2025-11-07
- Estimated Expiration
- 2045-03-25
AI Technical Summary
Existing nitrogen fertilizers have low utilization rates and short-lived effects, making it difficult to meet the fertilizer requirements of crops throughout their entire growth period. Furthermore, traditional urease inhibitors and nitrification inhibitors have unstable effects under different soil and climate conditions, high production costs, and may have negative impacts on soil microorganisms.
Active ingredients are further extracted from sewage treatment plant sludge and agricultural waste rice bran, and then rationally combined with other components to form a stable and efficient fertilizer synergist, including urease inhibitors, nitrification inhibitors, activators, modified sepiolite powder, and fatty alcohol polyoxyethylene ether, forming a 'fast-slow combined' nutrient supply system.
It significantly improves nitrogen fertilizer utilization, prolongs nutrient release time, improves soil environment, reduces production costs, reduces dependence on chemical raw materials, and promotes plant growth and root development.
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Figure CN120157553B_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The application belongs to the technical field of fertilizer synergists, and particularly relates to a fertilizer synergist and a preparation method thereof. BACKGROUND
[0002] Nitrogen fertilizer is an indispensable element for crop growth and is the main component of protein, chlorophyll and enzyme. Chemical nitrogen fertilizer mainly uses amide nitrogen fertilizer (urea). If crops lack nitrogen during growth, nitrogen fertilizer needs to be applied for compensation. However, there are the following technical problems in the use of nitrogen fertilizer by farmers: (1) low utilization rate of N; (2) short fertilizer efficiency, which is difficult to meet the fertilizer requirement characteristics of crops in the whole growth period, and multiple topdressing is necessary; (3) damage to soil and environment.
[0003] Urea, as a common nitrogen fertilizer, has a low utilization rate, usually only 30%-40%. In order to improve the utilization rate of urea, the existing technology has widely adopted methods such as adding urease inhibitors, nitrification inhibitors and the like to slow down the urea hydrolysis and nitrification process. Urease inhibitors can delay the process of urea hydrolysis into ammonium nitrogen by inhibiting urease activity, and reduce ammonia volatilization. Nitrification inhibitors can delay the conversion of ammonium nitrogen into nitrate nitrogen by inhibiting the activity of nitrifying bacteria, and reduce nitrification-denitrification loss and nitrate leaching. However, certain urease inhibitors (such as NBPT) are prone to decomposition under high temperature, high humidity or strong light conditions, resulting in a decline in their inhibitory effect; the effect of urease inhibitors is greatly affected by environmental factors such as soil pH, temperature and humidity, and their performance is inconsistent under different soil and climate conditions; high-efficiency urease inhibitors (such as NBPT) have high production costs, increasing the total cost of the fertilizer and possibly affecting its large-scale promotion; long-term and large-scale use of urease inhibitors may have a negative impact on soil microbial communities and destroy the ecological balance of the soil. The effect of nitrification inhibitors is also greatly affected by factors such as soil type, temperature and humidity. For example, DCD has a better effect under low temperature conditions, but it degrades faster under high temperature conditions; certain nitrification inhibitors (such as DCD) may remain in the soil for a long time, potentially affecting subsequent crops or soil microorganisms; high-efficiency nitrification inhibitors (such as DMPP and Nitrapyrin) have high production costs, limiting their widespread application in field crops. The use of urease inhibitors or nitrification inhibitors alone is difficult to comprehensively solve the problem of urea nitrogen loss, and the synergistic effect between the two has not been fully tapped. Therefore, it is a technical problem to be solved in the existing technology to provide a more efficient, more stable and more environmentally friendly fertilizer synergist to achieve the dual goals of nitrogen fertilizer efficiency and environmental protection. SUMMARY
[0004] The present application aims to provide a kind of fertilizer synergist, sewage treatment plant sludge and agricultural waste rice bran are further extracted active ingredients, and other components are reasonably matched to form stable and efficient fertilizer synergist, significantly reduce the use of chemical raw material type synergist, reduce production cost, improve nitrogen fertilizer utilization, promote plant growth, improve plant stress resistance.
[0005] To achieve the above technical purposes, the technical scheme adopted by the present application is:
[0006] A kind of fertilizer synergist, it is by urease inhibitor 0.1-0.3 parts, nitrification inhibitor 0.3-0.5 parts, active agent 5-10 parts, modified sepiolite powder 30-40 parts, fatty alcohol polyoxyethylene ether 5-8 parts composition;The active agent is sludge extract and rice bran extract according to 2:1 mass ratio composition.
[0007] Preferably, the sludge extract is prepared by the following method:
[0008] Step 1, take the remaining sludge and dry it to a moisture content of less than 10%, then crush it into sludge particles with a particle size of 1mm;
[0009] Step 2, take the sludge particles and mix them with a 3% sulfuric acid solution according to a ratio of 1g:5ml, heat to 80-90℃, stir for 3-4h, then solid-liquid separation, wash the solid to neutral to obtain filter residue I and acid hydrolysis liquid;
[0010] Step 3, take filter residue I and mix it with a 5% sodium hydroxide solution according to a ratio of 1g:5ml, heat to 90-100℃, stir for 3-4h, then solid-liquid separation, wash the solid to neutral to obtain filter residue II and alkali hydrolysis liquid;
[0011] Step 4, take filter residue II and add deionized water to it according to a ratio of 1g:10ml, stir evenly, then add 1.5wt% of a complex enzyme solution, heat to 55-60℃, then enzymatic hydrolysis for 3-4h, then terminate the enzyme, solid-liquid separation, to obtain filter residue III and enzymatic hydrolysis liquid;
[0012] Step 5, mix the acid hydrolysis liquid, alkali hydrolysis liquid and enzymatic hydrolysis liquid according to a volume ratio of 1:1:2 to obtain a mixed liquid, add 10% of activated carbon to the total weight to the mixed liquid, stir at room temperature for 1h, then filter to obtain the filtrate, further concentrate the filtrate to one tenth of the original volume, spray dry into powder to obtain the sludge extract.
[0013] Preferably, the remaining sludge is derived from a sewage treatment plant that uses biological methods to treat sewage.
[0014] Preferably, the complex enzyme solution in step 5 contains cellulase 30-40g / L, laccase 5-10g / L, and alpha-amylase 15-20g / L.
[0015] Preferably, the cellulase has an enzyme activity of 100,000 u / g, the laccase has an enzyme activity of 100,000 u / g, and the alpha-amylase has an enzyme activity of 30,000 u / g.
[0016] Preferably, the rice bran extract is prepared by the following method:
[0017] (1) Defatted rice bran is dissolved in deionized water at a solid-liquid ratio of 1:10, stirred at room temperature for 1 h, then the pH of the mixture is adjusted to 9-10 with NaOH, the mixture is heated to 50℃, and after magnetic stirring for 2 h, the supernatant is separated by centrifugation, 1 mol / L HCl solution is added to the supernatant to adjust the pH to 4.0, and after standing for 40-45 min, the solid is separated by centrifugation, the solid product is washed with deionized water for 3-4 times, and after drying, a solid product A is obtained.
[0018] (2) 1 g of the solid product A is dissolved in 100 ml of deionized water, and after mixing, neutral protease is added for enzymolysis at room temperature for 3-4 h, then the pH of the enzymolysis solution is adjusted to 6.0-6.5, and a composite enzyme is added for enzymolysis at 50-55℃ for 2-3 h, the enzymolysis solution is adjusted to neutral, centrifuged, and the supernatant is spray-dried into powder to obtain the rice bran extract.
[0019] Preferably, the composite enzyme is composed of papain and bromelain at a mass ratio of 2:1, the amount of the neutral protease is 1% of the mass of the solid product A, the amount of the composite enzyme is 1.5% of the mass of the solid product A, and the enzyme activity of the neutral protease, papain and bromelain is all 100,000 u / g.
[0020] Preferably, the modified sepiolite is prepared by the following method:
[0021] (a) Sepiolite powder is added to a 2 mol / L hydrochloric acid solution at a solid-liquid ratio of 1:15, heated to 80℃, and after magnetic stirring for 10 h, filtered, and the solid is repeatedly washed until the surface is neutral, and dried to obtain acid-modified sepiolite powder;
[0022] (b) The acid-modified sepiolite powder is mixed with a 1 mol / L ferrous chloride solution at a solid-liquid ratio of 1:10, magnetically stirred at room temperature for 1 h, and after standing for 24 h, filtered, and the solid precipitate is dried in an oven and ground into powder to obtain modified sepiolite powder.
[0023] Preferably, the urease inhibitor is N-butyl thiophosphoric triamide or N-propyl thiophosphoric triamide, and the nitrification inhibitor is dicyandiamide.
[0024] The application also provides a preparation method of the fertilizer synergist, which comprises the following steps:
[0025] S1: respectively preparing sludge extract and rice bran extract, and then preparing active agent according to mass ratio;
[0026] S2: preparing modified sepiolite powder;
[0027] S3: dissolving fatty alcohol polyoxyethylene ether in 10 times mass of water, then adding modified sepiolite powder and active agent component into the water, stirring and mixing at high speed for 30 min, then adding urease inhibitor and nitrification inhibitor, stirring and mixing uniformly, and then drying to obtain the fertilizer synergist.
[0028] The fertilizer synergist prepared by the application is used simultaneously with urea, and the usage amount is 2% of the mass of urea.
[0029] Residual sludge is the main by-product of the biological treatment process of sewage, and is regarded as waste in the traditional concept. In the process of global efforts to improve the performance of sewage treatment facilities and expand their coverage in developing countries, the sludge production continues to increase significantly, and the economic and environmental problems related to its treatment and disposal become increasingly prominent. The sludge contains various unique energy and nutrients, and if it can be reasonably utilized, the resource utilization rate can be improved. The sludge extract obtained after acid treatment, alkali treatment and enzyme treatment of the sludge contains various bioactive components such as polysaccharides, organic acids and amino acids secreted by microorganisms under specific conditions, and various trace element inorganic components such as calcium, magnesium and silicon; the active substances of the sludge extract have gel formation ability, and after the fertilizer is applied to the soil, they interact with the nutrients in the soil to form a stable matrix network, can adsorb more urea to form a stable complex, and further delay the hydrolysis of urea. At the same time, the organic matter in the sludge extract can provide a carbon source for soil microorganisms, promote the utilization of urea by microorganisms, reduce the direct hydrolysis of urea, and also can improve the soil structure, enhance the soil water and fertilizer retention capacity, and realize long-term slow release of nutrients. The rice bran extract prepared by the application is rich in small molecule peptides, amino acids, organic acids and other active ingredients, and can provide a rapid and effective nitrogen source for plants, promote the development of plant roots and nutrient absorption. The active agent prepared by the best ratio of the two in the application can meet the nutrient demand of plants at different growth stages, and improve the utilization rate of nitrogen fertilizer.
[0030] Urease inhibitors (such as N-butyl thiophosphoric triamide) can inhibit the activity of urease in the soil, slow down the hydrolysis rate of urea, and reduce the volatilization loss of ammonium nitrogen. Nitrification inhibitors (such as dicyandiamide) can inhibit the activity of nitrifying bacteria in the soil, slow down the conversion of ammonium nitrogen to nitrate nitrogen, and reduce the leaching loss and denitrification loss of nitrate nitrogen. The organic substances in the active agent prepared in the present application can form stable complexes with ammonium nitrogen, reducing the nitrification of ammonium nitrogen. At the same time, the organic substances in the active agent can provide carbon sources for soil microorganisms, promoting the immobilization of ammonium nitrogen by microorganisms and reducing the occurrence of nitrification.
[0031] The modified sepiolite powder can load urease inhibitors, nitrification inhibitors and active agents, prolong their action time, and improve the utilization rate of fertilizers. At the same time, the ferrous ions in the modified sepiolite powder and the active small molecule peptides in the active agent can interact to form stable chelates, further enhancing the slow-release effect of the fertilizer and providing more abundant nutrients for plants.
[0032] The fatty alcohol polyoxyethylene ether as a surfactant can improve the dispersibility and adsorbability of the fertilizer, enhance the permeability and stability of the fertilizer in the soil, and ensure the effect of the fertilizer synergist under different soil conditions.
[0033] Compared with the prior art, the present application has the following advantages:
[0034] (1) Through the synergistic effect of a small amount of urease inhibitors and nitrification inhibitors, the volatilization, nitrification-denitrification loss and leaching loss of urea nitrogen are reduced, and the utilization rate of nitrogen fertilizer is significantly improved. The combined use of the active agent, urease inhibitors and nitrification inhibitors in the present application can delay the hydrolysis of urea and the nitrification of ammonium nitrogen by the organic substances in the active agent, and further inhibit the volatilization and leaching loss of nitrogen by the urease inhibitors and nitrification inhibitors;
[0035] (2) The sludge extract and rice bran extract in the active agent not only provide nutrients for plants and prolong the release time of nutrients, but also improve the soil environment and promote the development of plant roots and nutrient absorption;
[0036] (3) The use of waste resources such as sludge and rice bran reduces the use of urease inhibitors and nitrification inhibitors, reduces production costs, reduces the dependence on chemically synthesized synergists, and has significant environmental benefits. BRIEF DESCRIPTION OF DRAWINGS
[0037] Figure 1 The test results of dry matter accumulation of corn aboveground in the test example of the present application;
[0038] Figure 2 The test results of ammonium nitrogen content in the soil of corn at the jointing stage and the mature stage in the test example of the present application;
[0039] Figure 3 The test results of the nitrate nitrogen content in the soil of the test corn of the present application at the jointing stage and the mature stage. DETAILED DESCRIPTION
[0040] The technical solutions of the present application are further described below in combination with specific examples, but are not limited thereto.
[0041] Example 1
[0042] A fertilizer synergist, which is composed of 0.1 parts of urease inhibitor, 0.3 parts of nitrification inhibitor, 5 parts of active agent, 30 parts of modified sepiolite powder and 5 parts of fatty alcohol polyoxyethylene ether; the active agent is composed of sludge extract and rice bran extract in a mass ratio of 2:1.
[0043] The sludge extract is prepared by the following method:
[0044] Step 1, dry the residual sludge to a water content of less than 10%, and then crush it into sludge particles with a particle size of 1 mm;
[0045] Step 2, mix the sludge particles with a 3% sulfuric acid solution in a ratio of 1g:5ml, heat to 80-90℃, and stir for 3-4h, then separate the solid and liquid, wash the solid to neutral to obtain filter residue I and acid hydrolysis liquid;
[0046] Step 3, mix the filter residue I with a 5% sodium hydroxide solution in a ratio of 1g:5ml, heat to 90-100℃, and stir for 3-4h, then separate the solid and liquid, wash the solid to neutral to obtain filter residue II and alkali hydrolysis liquid;
[0047] Step 4, add deionized water to the filter residue II in a ratio of 1g:10ml, stir evenly, then add 1.5wt% of a composite enzyme solution, heat to 55-60℃, and enzymatically hydrolyze for 3-4h, then terminate the enzyme, separate the solid and liquid, to obtain filter residue III and enzymatic hydrolysis liquid;
[0048] Step 5, mix the acid hydrolysis liquid, alkali hydrolysis liquid and enzymatic hydrolysis liquid in a ratio of 1:1:2 by volume to obtain a mixed liquid, add 10% of activated carbon based on the total weight to the mixed liquid, stir at room temperature for 1h, then filter to obtain the filtrate, further concentrate the filtrate to 1 / 10 of the original volume, and spray dry the powder to obtain the sludge extract.
[0049] The residual sludge is derived from a sewage treatment plant that uses a biological method to treat sewage.
[0050] The composite enzyme solution in step 5 contains cellulase 30g / L, laccase 5g / L and alpha-amylase 15g / L.
[0051] The cellulase has an enzyme activity of 100,000 u / g, the laccase has an enzyme activity of 100,000 u / g, and the alpha-amylase has an enzyme activity of 30,000 u / g.
[0052] The rice bran extract is prepared by the following method:
[0053] (1) Defatted rice bran is dissolved in deionized water at a solid-liquid ratio of 1:10, stirred at room temperature for 1 h, then the pH of the mixture is adjusted to 9-10 with NaOH, the mixture is heated to 50℃, and magnetically stirred for 2 h, then centrifugal separation is performed to obtain the supernatant, 1 mol / L HCl solution is added to the supernatant to adjust the pH to 4.0, and the mixture is left to stand for 40-45 min, then centrifugal separation is performed to obtain the solid, the solid product is washed with deionized water for 3-4 times, and then dried to obtain a solid product A;
[0054] (2) 1 g of the solid product A is dissolved in 100 ml of deionized water, mixed uniformly, then neutral protease is added and enzymolysis is performed at room temperature for 3-4 h, then the pH of the enzymolysis solution is adjusted to 6.0-6.5, a composite enzyme is added and enzymolysis is performed at 50-55℃ for 2-3 h, then the enzymolysis solution is adjusted to neutral, centrifugal separation is performed, and the supernatant is spray-dried to obtain a powder, which is the rice bran extract.
[0055] The composite enzyme is composed of papain and bromelain at a mass ratio of 2:1; the neutral protease is used in an amount of 1% of the mass of the solid product A, and the composite enzyme is used in an amount of 1.5% of the mass of the solid product A; the enzyme activity of the neutral protease, the papain and the bromelain is all 100,000 u / g.
[0056] The modified sepiolite is prepared by the following method:
[0057] (a) Sepiolite powder is added to a 2 mol / L hydrochloric acid solution at a solid-liquid ratio of 1:15, heated to 80℃, magnetically stirred for 10 h, then filtered, and the solid is repeatedly washed until the surface is neutral, and then dried to obtain acid-modified sepiolite powder;
[0058] (b) The acid-modified sepiolite powder is mixed with a 1 mol / L ferrous chloride solution at a solid-liquid ratio of 1:10, magnetically stirred at room temperature for 1 h, then left to stand for 24 h, then filtered, and the solid precipitate is dried in an oven and then ground into powder to obtain modified sepiolite powder.
[0059] The urease inhibitor is N-butyl thiophosphoric triamide; and the nitrification inhibitor is dicyandiamide.
[0060] A preparation method of the above-mentioned fertilizer synergist, which comprises the following steps:
[0061] S1: respectively preparing a sludge extract and a rice bran extract, and then composing an active agent according to a mass ratio;
[0062] S2: preparing modified sepiolite powder;
[0063] S3: dissolving fatty alcohol polyoxyethylene ether in 10 times mass of water, then adding modified sepiolite powder and active agent component, mixing for 30 min under high speed stirring, then adding urease inhibitor and nitrification inhibitor, mixing uniformly, drying to obtain the fertilizer synergist.
[0064] Example 2
[0065] A fertilizer synergist, which is composed of urease inhibitor 0.3 parts, nitrification inhibitor 0.5 parts, active agent 10 parts, modified sepiolite powder 40 parts, and fatty alcohol polyoxyethylene ether 8 parts; the active agent is composed of sludge extract and rice bran extract according to a mass ratio of 2:1.
[0066] The sludge extract is prepared by the following method:
[0067] Step 1: drying the residual sludge to a water content of less than 10%, then crushing into sludge particles with a particle size of 1 mm;
[0068] Step 2: mixing the sludge particles with 3% sulfuric acid solution according to a ratio of 1 g:5 ml, heating to 80-90℃, stirring for 3-4 h, then solid-liquid separation, washing the solid to neutral to obtain filter residue I and acid hydrolysis liquid;
[0069] Step 3: mixing filter residue I with 5% sodium hydroxide solution according to a ratio of 1 g:5 ml, heating to 90-100℃, stirring for 3-4 h, then solid-liquid separation, washing the solid to neutral to obtain filter residue II and alkali hydrolysis liquid;
[0070] Step 4: adding deionized water to filter residue II according to a ratio of 1 g:10 ml, stirring uniformly, then adding 1.5 wt% of a composite enzyme solution, heating to 55-60℃, and enzymatic hydrolysis for 3-4 h, then enzyme inactivation, solid-liquid separation, to obtain filter residue III and enzymatic hydrolysis liquid;
[0071] Step 5: mixing the acid hydrolysis liquid, alkali hydrolysis liquid, and enzymatic hydrolysis liquid according to a volume ratio of 1:1:2 to obtain a mixed liquid, adding 10% of activated carbon based on the total weight to the mixed liquid, stirring for 1 h at room temperature, then filtering to obtain the filtrate, further concentrating the filtrate to 1 / 10 of the original volume, and spray drying to obtain the sludge extract.
[0072] The residual sludge is derived from a sewage treatment plant using a biological method to treat sewage.
[0073] The composite enzyme solution in step 5 contains cellulase 40 g / L, laccase 10 g / L, and alpha-amylase 20 g / L.
[0074] The cellulase has an enzyme activity of 100,000 u / g, the laccase has an enzyme activity of 100,000 u / g, and the alpha-amylase has an enzyme activity of 30,000 u / g.
[0075] The rice bran extract is prepared by the following method:
[0076] (1) Defatted rice bran is dissolved in deionized water at a solid-liquid ratio of 1:10, stirred at room temperature for 1 h, then the pH of the mixture is adjusted to 9-10 with NaOH, the mixture is heated to 50℃, and after magnetic stirring for 2 h, the supernatant is separated by centrifugation, 1 mol / L HCl solution is added to the supernatant to adjust the pH to 4.0, and after standing for 40-45 min, the solid is separated by centrifugation, the solid product is washed with deionized water for 3-4 times, and after drying, a solid product A is obtained;
[0077] (2) 1 g of the solid product A is dissolved in 100 ml of deionized water, mixed uniformly, then neutral protease is added for enzymolysis at room temperature for 3-4 h, the pH of the enzymolysis solution is adjusted to 6.0-6.5, and then a composite enzyme is added for enzymolysis at 50-55℃ for 2-3 h to inactivate the enzyme, the enzymolysis solution is adjusted to neutral, centrifuged, and the supernatant is spray-dried into powder to obtain the rice bran extract.
[0078] The composite enzyme is composed of papain and bromelain at a mass ratio of 2:1; the amount of the neutral protease is 1% of the mass of the solid product A, and the amount of the composite enzyme is 1.5% of the mass of the solid product A; the enzyme activity of the neutral protease, papain and bromelain is all 100,000 u / g.
[0079] The modified sepiolite is prepared by the following method:
[0080] (a) Sepiolite powder is added to a 2 mol / L hydrochloric acid solution at a solid-liquid ratio of 1:15, heated to 80℃, and after magnetic stirring for 10 h, filtered, and the solid is repeatedly washed until the surface is neutral, and then dried to obtain acid-modified sepiolite powder;
[0081] (b) The acid-modified sepiolite powder is mixed with a 1 mol / L ferrous chloride solution at a solid-liquid ratio of 1:10, magnetically stirred at room temperature for 1 h, and after standing for 24 h, filtered, and the solid precipitate is dried in an oven and ground into powder to obtain modified sepiolite powder.
[0082] The urease inhibitor is N-butyl thiophosphoric triamide or N-propyl thiophosphoric triamide; and the nitrification inhibitor is dicyandiamide.
[0083] A preparation method of the above-mentioned fertilizer synergist, which comprises the following steps:
[0084] S1: separately preparing a sludge extract and a rice bran extract, and then composing an active agent according to a mass ratio;
[0085] S2: preparing modified sepiolite powder;
[0086] S3: dissolving fatty alcohol polyoxyethylene ether in 10 times mass of water, then adding modified sepiolite powder and active agent component, mixing for 30 min under high speed stirring, then adding urease inhibitor and nitrification inhibitor, mixing uniformly, drying to obtain the fertilizer synergist.
[0087] Example 3
[0088] A fertilizer synergist, which is composed of urease inhibitor 0.2 parts, nitrification inhibitor 0.4 parts, active agent 8 parts, modified sepiolite powder 35 parts, and fatty alcohol polyoxyethylene ether 6 parts; the active agent is composed of sludge extract and rice bran extract according to a mass ratio of 2:1.
[0089] The sludge extract is prepared by the following method:
[0090] Step 1: drying the residual sludge to a water content of less than 10%, then crushing into sludge particles with a particle size of 1 mm;
[0091] Step 2: mixing the sludge particles with 3% sulfuric acid solution according to a ratio of 1 g:5 ml, heating to 80-90℃, stirring for 3-4 h, then solid-liquid separation, washing the solid to neutral to obtain filter residue I and acid hydrolysis liquid;
[0092] Step 3: mixing filter residue I with 5% sodium hydroxide solution according to a ratio of 1 g:5 ml, heating to 90-100℃, stirring for 3-4 h, then solid-liquid separation, washing the solid to neutral to obtain filter residue II and alkali hydrolysis liquid;
[0093] Step 4: adding deionized water to filter residue II according to a ratio of 1 g:10 ml, stirring uniformly, then adding 1.5 wt% of a complex enzyme solution, heating to 55-60℃, and enzymatic hydrolysis for 3-4 h, then enzyme inactivation, solid-liquid separation, to obtain filter residue III and enzymatic hydrolysis liquid;
[0094] Step 5: mixing the acid hydrolysis liquid, alkali hydrolysis liquid, and enzymatic hydrolysis liquid according to a volume ratio of 1:1:2 to obtain a mixed liquid, adding 10% of activated carbon based on the total weight to the mixed liquid, stirring for 1 h at room temperature, then filtering to obtain the filtrate, further concentrating the filtrate to 1 / 10 of the original volume, and spray drying to obtain the sludge extract.
[0095] The residual sludge is derived from a sewage treatment plant using a biological method to treat sewage.
[0096] The complex enzyme solution in step 5 contains cellulase 35 g / L, laccase 8 g / L, and alpha-amylase 16 g / L.
[0097] The cellulase has an enzyme activity of 100,000 u / g, the laccase has an enzyme activity of 100,000 u / g, and the alpha-amylase has an enzyme activity of 30,000 u / g.
[0098] The rice bran extract is prepared by the following method:
[0099] (1) Defatted rice bran is dissolved in deionized water at a solid-liquid ratio of 1:10, stirred at room temperature for 1 h, then the pH of the mixture is adjusted to 9-10 with NaOH, the mixture is heated to 50℃, and magnetically stirred for 2 h, then centrifugal separation is performed to obtain the supernatant, 1 mol / L HCl solution is added to the supernatant to adjust the pH to 4.0, and the mixture is left to stand for 40-45 min, then centrifugal separation is performed to obtain the solid, the solid product is washed with deionized water for 3-4 times, and then dried to obtain a solid product A;
[0100] (2) 1 g of the solid product A is dissolved in 100 ml of deionized water, mixed uniformly, then neutral protease is added and enzymolysis is performed at room temperature for 3-4 h, then the pH of the enzymolysis solution is adjusted to 6.0-6.5, a composite enzyme is added and enzymolysis is performed at 50-55℃ for 2-3 h, then the enzymolysis solution is adjusted to neutral, centrifugal separation is performed, and the supernatant is spray-dried to obtain a rice bran extract.
[0101] The composite enzyme is composed of papain and bromelain at a mass ratio of 2:1; the neutral protease is used in an amount of 1% of the mass of the solid product A, and the composite enzyme is used in an amount of 1.5% of the mass of the solid product A; the enzyme activity of the neutral protease, the papain and the bromelain is all 100,000 u / g.
[0102] The modified sepiolite is prepared by the following method:
[0103] (a) Sepiolite powder is added to a 2 mol / L hydrochloric acid solution at a solid-liquid ratio of 1:15, heated to 80℃, and magnetically stirred for 10 h, then filtered, and the solid is repeatedly washed until the surface is neutral, and then dried to obtain acid-modified sepiolite powder;
[0104] (b) The acid-modified sepiolite powder is mixed with a 1 mol / L ferrous chloride solution at a solid-liquid ratio of 1:10, magnetically stirred at room temperature for 1 h, then left to stand for 24 h, then filtered, and the solid precipitate is dried in an oven and then ground into powder to obtain modified sepiolite powder.
[0105] The urease inhibitor is N-propyl thiophosphoric triamide; and the nitrification inhibitor is dicyandiamide.
[0106] A preparation method of the fertilizer synergist, comprising the following steps:
[0107] S1: preparing a sludge extract and a rice bran extract respectively, and then composing an active agent according to a mass ratio;
[0108] S2: Preparation of modified sepiolite powder;
[0109] S3: Dissolve the fatty alcohol polyoxyethylene ether in 10 times the mass of water, then add the modified sepiolite powder and active agent component, mix at high speed for 30 min, then add the urease inhibitor and nitrification inhibitor, mix uniformly, dry, and obtain the fertilizer synergist.
[0110] Comparative Example 1
[0111] A fertilizer synergist, which has the same basic principle and composition as Example 3, except that the active agent only contains sludge extract.
[0112] Comparative Example 2
[0113] A fertilizer synergist, which has the same basic principle and composition as Example 3, except that the active agent only contains rice bran extract.
[0114] Comparative Example 3
[0115] A fertilizer synergist, which has the same basic principle and composition as Example 3, except that it does not contain an active agent.
[0116] Comparative Example 4
[0117] A fertilizer synergist, which has the same basic principle and composition as Example 3, except that it does not contain the urease inhibitor N-propyl thiophosphoric triamide.
[0118] Comparative Example 5
[0119] A fertilizer synergist, which has the same basic principle and composition as Example 3, except that it does not contain the nitrification inhibitor dicyandiamide.
[0120] Comparative Example 6
[0121] A fertilizer synergist, which has the same basic principle and composition as Example 3, except that it does not contain the nitrification inhibitor dicyandiamide and the urease inhibitor N-propyl thiophosphoric triamide.
[0122] Test Example
[0123] Test site: Choose Shikofeng Agricultural Planting Test Base in Linyi Economic Development Zone, Shandong Province, soil type is loam, fertility is medium. The basic physicochemical properties of 0-20 cm soil are: pH value 5.89, organic matter 20.89 g / kg, alkali-hydrolyzable nitrogen 93.9 mg / kg, available phosphorus 23.4 mg / kg, and available potassium 208 mg / kg.
[0124] Test crop variety: corn, Xianyu 335, planting density is 4000 plants per mu. Planting time is in the middle and late June every year, and harvesting is in the middle of October.
[0125] Test design: 9 treatment groups were set in this test, 1-9 treatment groups, wherein 1 is the treatment group of example 3, 2-7 is the treatment group of comparative examples 1-6, 8 is the conventional fertilizer control group without using any synergist, and 9 is the control group without applying any nitrogen fertilizer. The test plot area is 45 m 2 , each treatment is repeated 3 times, and the experimental results are averaged. All treatment groups of fertilizers are one-time base application, and the fertilizer application amount is N 200 kg / hm 2 , P2O5 100 kg / hm 2 , K2O 100 kg / hm 2 , nitrogen fertilizer, phosphorus fertilizer and potassium fertilizer are respectively provided by urea (containing N 46%), heavy superphosphate (P2O5 45%) and potassium sulfate (K2O 60%). The amount of fertilizer synergist is 2% of the mass of urea, which is uniformly mixed with urea and also applied as base fertilizer once, and is buried into the soil after being spread and buried. Other field management measures are the same as the local conventional management.
[0126] Test items and methods:
[0127] Dry matter accumulation of aboveground part: at the mature stage, 10 representative plants are selected in each treatment, killed at 105℃ for 30 min, dried at 80℃ to constant weight, and weighed to calculate the dry matter accumulation of aboveground part. As shown in Figure 1 .
[0128] As can be seen from Figure 1 , the dry matter accumulation of corn in example 3 of the present application is significantly higher than that in other comparative examples, which shows that the use of the fertilizer synergist prepared by the present application can significantly promote the accumulation of dry matter of corn.
[0129] At the jointing stage and the mature stage, 20 g of 0~20 cm plough layer soil is taken from each plot by 5-point sampling method, the soil samples are mixed, impurities are removed, sieved and then respectively packed into self-sealing bags, and stored at-20℃. The soil samples are extracted with 1 M KCL solution, and then the content of ammonium nitrogen (NH4 + -N) and nitrate nitrogen (NO3 - -N) of the soil is determined by AA3 type continuous flow analyzer. The results are shown in Figure 2 and Figure 3 . As can be seen from Figure 2 and Figure 3 , with the growth of corn, both ammonium nitrogen and nitrate nitrogen show a decreasing trend from the jointing stage to the mature stage, which reflects that the absorption and utilization of nitrogen by corn is close to completion after the mature stage. Figure 2 As can be seen from the data in Figure 2 , the ammonium nitrogen content of example 3 is significantly higher than that of comparative examples 1-6, which shows that the treatment of adding the fertilizer synergist of example 3 of the present application can increase the ammonium nitrogen content in the soil at the jointing stage of corn, and maintain the ammonium nitrogen content in the soil at a certain level in the later period.Figure 3 As can be seen from the above Table 1, the nitrate nitrogen content in Example 3 is significantly lower than that in other comparative examples, which indicates that the addition of the fertilizer synergist treatment reduces the nitrate nitrogen content and reduces the risk of leaching of nitrate nitrogen to deep soil.
[0130] After drying the dry matter at the mature stage, grinding with a grinder, taking 0.2 g of the ground plant sample, decomposing with H2SO4-H2O2, diluting the digestion solution, and determining the total nitrogen content of the plant with an AA3 type continuous flow analyzer, the relevant indexes are calculated:
[0131] Nitrogen fertilizer partial productivity (PFPN, kg / kg) = yield / nitrogen application amount;
[0132] Nitrogen fertilizer agronomic efficiency (NAE, kg / kg) = (yield of nitrogen application treatment - yield of no nitrogen application treatment) / nitrogen application amount;
[0133] Nitrogen fertilizer utilization rate (NUE, %) = (nitrogen uptake amount of nitrogen application treatment - nitrogen uptake amount of no nitrogen application treatment) / nitrogen application amount x 100. As shown in Table 1.
[0134] Table 1 Effect of fertilizer synergist of different treatment groups on nitrogen utilization efficiency of corn
[0135]
[0136] As can be seen from the above Table 1, the fertilizer synergist of Example 3 of the present application can significantly improve the nitrogen fertilizer utilization rate, and the effect is better than that of other comparative examples. Comparative examples 1-6 change the raw material composition of the present application, and the corresponding effect is poor, which indicates that the raw material composition and the ratio of the present application are complementary and indispensable.
[0137] Harvest at the mature stage, randomly select 30 ears from each plot, investigate yield trait indexes, examine ear length, ear thickness, bare tip length, ear row number, row grain number, thousand grain weight, and ear grain weight. The statistical results are shown in Table 2.
[0138] Table 2 Corn yield and constituent factors of different treatments
[0139]
[0140] It should be noted that the above examples are only part of the preferred modes of implementing the present application, not all. Obviously, based on the above examples of the present application, all other examples obtained by those of ordinary skill in the art without creative labor should be within the scope of protection of the present application.
Claims
1. A fertilizer synergist, characterized in that, It is composed of urease inhibitor 0.1-0.3 parts, nitration inhibitor 0.3-0.5 parts, active agent 5-10 parts, modified sepiolite powder 30-40 parts, fatty alcohol polyoxyethylene ether 5-8 parts; the active agent is sludge extract and rice bran extract in a mass ratio of 2:1; the sludge extract is prepared by the following method: Step 1, after the remaining sludge is dried to a water content of less than 10%, it is crushed into sludge particles with a particle size of 1mm; Step 2, take the sludge particles and mix them with a 3% sulfuric acid solution in a ratio of 1g:5ml, heat to 80-90℃, stir for 3-4h, then separate the solid and liquid, wash the solid to neutral to obtain filter residue I and acid hydrolysis liquid; Step 3, take filter residue I and mix it with a 5% sodium hydroxide solution in a ratio of 1g:5ml, heat to 90-100℃, stir for 3-4h, then separate the solid and liquid, wash the solid to neutral to obtain filter residue II and alkali hydrolysis liquid; Step 4, take filter residue II and add deionized water to it in a ratio of 1g:10ml, stir evenly, then add 1.5wt% of a composite enzyme solution, heat to 55-60℃, and enzymatically hydrolyze for 3-4h, then terminate the enzyme, separate the solid and liquid, to obtain filter residue III and enzymatic hydrolysis liquid; Step 5, mix the acid hydrolysis liquid, alkali hydrolysis liquid, and enzymatic hydrolysis liquid in a volume ratio of 1:1:2 to obtain a mixed liquid, add 10% of active carbon to the total weight to the mixed liquid, stir at room temperature for 1h, then filter to obtain the filtrate, further concentrate the filtrate to one tenth of the original volume, and spray dry the powder to obtain the sludge extract; The rice bran extract is prepared by the following method: (1) dissolve the defatted rice bran in deionized water at a solid-liquid ratio of 1:10, stir at room temperature for 1h, then adjust the pH of the mixed liquid to 9-10 with NaOH, heat the mixed liquid to 50℃, magnetically stir for 2h, then centrifugally separate to obtain the supernatant, add 1 mol / L HCl solution to the supernatant to adjust the pH to 4.0, stand for 40-45min, then centrifugally separate to obtain the solid, wash the solid product with deionized water for 3-4 times, and dry to obtain solid A; (2) dissolve 1g of solid A in 100ml of deionized water, mix evenly, then add neutral protease to the mixture, enzymatically hydrolyze at room temperature for 3-4h, then adjust the pH of the enzymatic hydrolysis liquid to 6.0-6.5, add a composite enzyme to the mixture, and enzymatically hydrolyze at 50-55℃ for 2-3h to terminate the enzyme, adjust the enzymatic hydrolysis liquid to neutral, centrifugally separate, take the supernatant, and spray dry the powder to obtain the rice bran extract.
2. The fertilizer synergist of claim 1, wherein, The remaining sludge is derived from a sewage treatment plant that uses a biological method to treat sewage.
3. The fertilizer performance enhancer of claim 1, wherein, The composite enzyme solution in step 5 contains cellulase 30-40g / L, laccase 5-10g / L, and alpha-amylase 15-20g / L.
4. The fertilizer performance enhancer of claim 3, wherein, The cellulase has an enzyme activity of 100,000u / g, the laccase has an enzyme activity of 100,000u / g, and the alpha-amylase has an enzyme activity of 30,000u / g.
5. The fertilizer performance enhancer of claim 1, wherein, The complex enzyme is composed of papain and bromelain in a mass ratio of 2:1; the neutral protease is used in an amount of 1% of the solid A, and the complex enzyme is used in an amount of 1.5% of the solid A; the enzyme activity of the neutral protease, papain and bromelain is all 100,000 u / g.
6. The fertilizer enhancer of claim 1, wherein, The modified sepiolite is prepared by the following method: (a) sepiolite powder is added into 2 mol / L hydrochloric acid solution in a solid-liquid ratio of 1:15, heated to 80℃, and reacted for 10 h under magnetic stirring, then filtered, the solid is repeatedly washed until the surface is neutral, and dried to obtain acid-modified sepiolite powder; (b) the acid-modified sepiolite powder is mixed with 1 mol / L ferrous chloride solution in a solid-liquid ratio of 1:10, and reacted for 1 h under magnetic stirring at room temperature, then filtered after standing for 24 h, and the solid precipitate is dried in an oven and ground into powder to obtain modified sepiolite powder.
7. The fertilizer performance enhancer of claim 1, wherein, The urease inhibitor is N-butyl thiophosphoric triamide or N-propyl thiophosphoric triamide; and the nitrification inhibitor is dicyandiamide.
8. A method of preparing the fertilizer efficiency agent of any one of claims 1-7, characterized in that, It comprises the following steps: S1: preparing sludge extract and rice bran extract respectively, and then composing active agent according to mass ratio; S2: preparing modified sepiolite powder; S3: dissolving fatty alcohol polyoxyethylene ether in 10 times mass of water, then adding modified sepiolite powder and active agent components into the water, mixing under high-speed stirring for 30 min, then adding urease inhibitor and nitrification inhibitor, and mixing uniformly, and then drying to obtain fertilizer synergist.
Citation Information
Patent Citations
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