CN115894113A - Composite active slow-release liquid fertilizer and preparation method thereof - Google Patents
Composite active slow-release liquid fertilizer and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a composite active slow-release liquid fertilizer which is prepared from the following components in parts by weight: 200-300 parts of seaweed essence diluent, 50-160 parts of sodium carboxymethylcellulose solution, 15-20 parts of medical stone, 1~3 parts of theasaponin, 1~3 parts of kaline, 0.01-0.05 part of titanium dioxide, 20-30 parts of gamma-polyglutamic acid, 200-300 parts of deionized water and 5-15 parts of ethylene glycol diglycidyl ether; the preparation method of the compound active slow-release liquid fertilizer comprises the following steps: preparing a sodium carboxymethylcellulose solution and a seaweed essence diluent for later use; adding medical stone into citric acid solution, and reacting to obtain carboxylated medical stone; mixing carboxylated medical stone with titanium dioxide, theasaponin and kaline, and reacting to obtain modified medical stone; mixing gamma-polyglutamic acid solution and sodium carboxymethylcellulose solution, adding ethylene glycol diglycidyl ether and modified medical stone, fully reacting, grinding and crushing the product, adding the product into the seaweed essence diluent, and performing ultrasonic treatment to obtain the composite active slow-release liquid fertilizer.
Description
Technical Field
The invention relates to the field of fertilizer preparation, in particular to a compound active slow-release liquid fertilizer and a preparation method thereof.
Background
The seaweed is a lower organism growing in the sea, is a primary producer of a marine ecosystem, has a simple cell structure, a high growth speed and large individual size difference, and is diversified; the seaweed has low content of nitrogen and phosphorus, contains abundant inorganic elements and dozens of macroelements and trace elements in the seawater; the seaweed also contains active ingredients such as rare earth elements, phenolic compounds, growth regulating substances and the like which have the effect of promoting the growth and development of plants; phenolic compounds in the seaweed have an inhibiting effect on the growth of certain fungi, and the antioxidant property of the phenolic compounds is also beneficial to the preservation and storage of crops; the mannitol in the seaweed can chelate mineral elements to increase the content of nutrients available for plants, and the enzymes can promote the propagation of effective microorganisms in soil, thereby improving the physicochemical properties of the soil and increasing the soil fertility.
Chinese patent document CN201010106874.7 discloses an organic liquid fertilizer containing a biomass active extract component, which has various biological activities and functions, not only can provide comprehensive nutrition for plants, but also has the effects of bacteriostasis, sterilization, insect expelling, disinsection and plant growth regulation; the field test shows that the organic liquid fertilizer not only has obvious effect of increasing the yield of agricultural products, but also improves the quality of the agricultural products.
However, after the common fertilizer is applied, if the common fertilizer is not rained, a large amount of evaporation is caused, if the rainwater is too large, the fertilizer is lost along with water, and a large amount of waste of the fertilizer and manpower is caused, so that the liquid fertilizer with the slow release effect needs to be provided, and the fertilizer effect and the insecticidal effect can be provided for a long time.
Disclosure of Invention
In order to solve the defects in the prior art, the invention aims to provide a compound active slow-release liquid fertilizer and a preparation method thereof, which can release nutrient substances and insecticidal substances for a long time, improve the effect of the fertilizer and the insecticide, improve the soil environment and restore heavy metal pollution in soil.
In order to achieve the purpose, the invention adopts the following technical scheme:
the composite active slow-release liquid fertilizer is prepared from the following components in parts by weight:
preferably, the compound active slow-release liquid fertilizer is prepared from the following components in parts by weight:
further preferably, the compound active slow-release liquid fertilizer is prepared from the following components in parts by weight:
preferably, the preparation method of the seaweed essence diluent comprises the following steps: mixing refined seaweed and deionized water according to the proportion of 1: mixing evenly 10-20 weight ratio to obtain the seaweed essence diluent.
Preferably, the preparation method of the sodium carboxymethyl cellulose solution is as follows: mixing sodium carboxymethylcellulose and deionized water according to the proportion of 1: uniformly mixing 8-15 weight percent to obtain the sodium carboxymethyl cellulose solution.
The invention also claims a preparation method of the compound active slow-release liquid fertilizer, which comprises the following steps:
(1) Adding medical stone into citric acid solution, washing and drying after reaction to obtain carboxylated medical stone;
(2) Mixing the carboxylated medical stone obtained in the step (1) with titanium dioxide, theasaponin and kaline, cooling and crushing after reaction, and sieving with a 200-300-mesh sieve to obtain modified medical stone;
(3) Dissolving gamma-polyglutamic acid in deionized water to obtain a gamma-polyglutamic acid solution, mixing the gamma-polyglutamic acid solution with a sodium carboxymethylcellulose solution, adding ethylene glycol diglycidyl ether and the modified medical stone obtained in the step (2), and washing, freezing and drying after reaction for later use;
(4) And (4) grinding the product obtained in the step (3) into powder, then adding the powder into the seaweed essence diluent, and carrying out ultrasonic treatment to obtain the composite active slow-release liquid fertilizer.
Preferably, in the step (1), the mass fraction of the citric acid solution is 10-20 g/L; the reaction condition is that the mixture is stirred for 5 to 10 hours at the temperature of between 60 and 90 ℃ and the rotating speed is between 200 and 300r/min.
Preferably, in the step (2), the reaction condition is that the mixture is heated to 200-250 ℃ under the protection of nitrogen and the reaction time is 8-12 h.
Preferably, in the step (3), the reaction condition is that the crosslinking is carried out for 36 to 48 hours at a temperature of between 30 and 60 ℃.
Preferably, in the step (4), the ultrasonic treatment is carried out for 5 to 8 hours at the ultrasonic power of 60 to 100W and the frequency of 17 to 22 kHz.
Compared with the prior art, the invention has the following beneficial effects:
1) The invention uses citric acid to activate medical stone, obviously increases the-COOH number on the surface of the medical stone, and then adds alkaloid insecticide tea saponin and kaline to the carboxylated medical stone through esterification and crosslinking reaction, so that the medical stone can slowly and durably release the alkaloid insecticide, the action time and the use effect of the insecticide are improved, and the disease-resistant and insect-repellent effects of the liquid fertilizer are prolonged.
2) The medical stone contains macroelements such as potassium, sodium, calcium, magnesium, phosphorus and the like and medium and trace elements such as zinc, iron, selenium, copper, strontium, iodine, fluorine and the like, can improve the physical and chemical properties of soil, increase the content of nutrient substances in the soil, promote the growth and development of plant rhizosphere and the activity of microorganisms, is a good soil conditioner, and particularly has remarkable improvement and recovery functions on hardened soil caused by continuous year cultivation and long-term use of fertilizers and soil with nutrient deficiency, pollution, fertilizer damage and the like caused by continuous cropping planting.
3) The sodium hydroxymethyl cellulose contains a large amount of hydroxyl, ether oxygen and carbonyl, can form hydrogen bonds and ionic bonds with carboxyl and amino in gamma-polyglutamic acid, and forms a three-dimensional interpenetrating network structure after being crosslinked with the gamma-polyglutamic acid, so that the modified zeolite can be loaded, the dissolution, storage, transportation and absorption of nutrient substances in the liquid fertilizer can be effectively improved, and the nutrient substances in the liquid fertilizer can be slowly released, thereby reducing the nutrient loss and reducing the liquid fertilizer material consumption.
4) The sodium carboxymethylcellulose and the gamma-polyglutamic acid cooperatively form a porous reticular structure, the medical stone loaded on the porous reticular structure has rich reticular structures, and the three substances contain rich functional groups, have a good adsorption effect on heavy metal ions, and can perform good conditioning and improving effects on soil.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. Of course, the specific embodiments described herein are merely illustrative of the invention and are not intended to be limiting.
The seaweed is purchased from Shandong Hongshengda chemical Co Ltd;
sodium carboxymethylcellulose was purchased from jonan element chemical limited, CAS:9085-26-1;
ethylene glycol diglycidyl ether was purchased from san-feida chemical co, suzhou, CAS:108-94-1;
gamma-polyglutamic acid was purchased from jateur bio-technologies ltd, jiang: 25513-46-6;
theasaponin was purchased from jonan xin chemical technology ltd, CAS:11006 to 75 to 0;
kaline was purchased from Hubeixin Hongli chemical Co., ltd, CAS:20562-03-2.
Example 1
A preparation method of a composite active slow-release liquid fertilizer comprises the following steps:
(1) Adding 50g of sodium carboxymethylcellulose into 500mL of deionized water, and uniformly stirring to obtain a sodium carboxymethylcellulose solution for later use;
(2) Adding 100g of seaweed essence into 2000mL of deionized water, and uniformly stirring to obtain seaweed essence diluent for later use;
(3) Adding 150g of medical stone into 1000mL of 10g/L citric acid solution, stirring at 60 ℃ and the rotation speed of 200r/min for 5 hours, washing after reaction, and drying to obtain carboxylated medical stone; mixing the obtained carboxylated medical stone with 0.1g of titanium dioxide, 10g of theasaponin and 10g of kaline, heating to 200 ℃ under the protection of nitrogen, reacting for 8 hours, cooling and crushing after the reaction, and sieving with a 200-mesh sieve to obtain modified medical stone;
(4) Dissolving 200g of gamma-polyglutamic acid in 2000mL of deionized water to obtain a gamma-polyglutamic acid solution, mixing the gamma-polyglutamic acid solution with the sodium carboxymethylcellulose solution obtained in the step (1), adding 50g of ethylene glycol diglycidyl ether and the modified medical stone obtained in the step (3), crosslinking for 36 hours at 30 ℃, washing, freezing and drying after reaction for later use;
(5) Grinding the product obtained in the step (4) into powder, then adding the powder into the seaweed essence diluent obtained in the step (2), and carrying out ultrasonic treatment for 5 hours at 60W and 17kHz to obtain the compound active slow-release liquid fertilizer.
Example 2
A preparation method of a composite active slow-release liquid fertilizer comprises the following steps:
(1) Adding 100g of hydroxymethyl sodium carboxymethyl cellulose into 1500mL of deionized water, and uniformly stirring to obtain a hydroxymethyl sodium cellulose solution for later use;
(2) Adding 100g of seaweed essence into 3000mL of deionized water, and uniformly stirring to obtain a seaweed essence diluent for later use;
(3) Adding 200g of medical stone into 2000mL of 20g/L citric acid solution, stirring at 90 ℃ and the rotating speed of 300r/min for 10 hours, washing after reaction, and drying to obtain carboxylated medical stone; mixing the obtained carboxylated medical stone with 0.5g of titanium dioxide, 30g of theasaponin and 30g of kaline, heating to 250 ℃ under the protection of nitrogen, reacting for 12 hours, cooling and crushing after reaction, and sieving with a 300-mesh sieve to obtain modified medical stone;
(4) Dissolving 300g of gamma-polyglutamic acid in 3000mL of deionized water to obtain a gamma-polyglutamic acid solution, mixing the gamma-polyglutamic acid solution with the sodium carboxymethylcellulose solution obtained in the step (1), adding 150g of ethylene glycol diglycidyl ether and the modified medical stone obtained in the step (3), crosslinking for 48 hours at 60 ℃, washing, freezing and drying after reaction for later use;
(5) Grinding the product obtained in the step (4) into powder, then adding the powder into the seaweed essence diluent obtained in the step (2), and carrying out ultrasonic treatment for 8 hours at 100W and 22kHz to obtain the compound active slow-release liquid fertilizer.
Example 3
A preparation method of a composite active slow-release liquid fertilizer comprises the following steps:
(1) Adding 80g of sodium carboxymethylcellulose into 1000mL of deionized water, and uniformly stirring to obtain a sodium carboxymethylcellulose solution for later use;
(2) Adding 300g of seaweed essence into 3000mL of deionized water, and uniformly stirring to obtain seaweed essence diluent for later use;
(3) Adding 200g of medical stone into 1500mL of 15g/L citric acid solution, stirring at 80 ℃ and 250r/min for 8 hours, washing after reaction, and drying to obtain carboxylated medical stone; mixing the obtained carboxylated medical stone with 0.3g of titanium dioxide, 20g of theasaponin and 20g of kaline, heating to 220 ℃ under the protection of nitrogen, reacting for 10 hours, cooling and crushing after reaction, and sieving with a 250-mesh sieve to obtain modified medical stone;
(4) Dissolving 250g of gamma-polyglutamic acid in 2000mL of deionized water to obtain a gamma-polyglutamic acid solution, mixing the gamma-polyglutamic acid solution with the sodium hydroxymethyl cellulose solution obtained in the step (1), adding 100g of ethylene glycol diglycidyl ether and the modified medical stone obtained in the step (3), crosslinking for 42 hours at 40 ℃, reacting, washing, freezing and drying for later use;
(5) Grinding the product obtained in the step (4) into powder, then adding the powder into the seaweed essence diluent obtained in the step (2), and carrying out ultrasonic treatment for 6 hours at 80W and 20kHz to obtain the composite active slow-release liquid fertilizer.
Example 4
A preparation method of a composite active slow-release liquid fertilizer comprises the following steps:
(1) Adding 80g of sodium carboxymethylcellulose into 1200mL of deionized water, and uniformly stirring to obtain a sodium carboxymethylcellulose solution for later use;
(2) Adding 200g of seaweed essence into 3000mL of deionized water, and uniformly stirring to obtain seaweed essence diluent for later use;
(3) Adding 150g of medical stone into 1000mL of 10g/L citric acid solution, stirring at 70 ℃ and the rotation speed of 200r/min for 7 hours, washing after reaction, and drying to obtain carboxylated medical stone; mixing the obtained carboxylated medical stone with 0.2g of titanium dioxide, 10g of theasaponin and 20g of kaline, heating to 240 ℃ under the protection of nitrogen, reacting for 10 hours, cooling and crushing after the reaction, and sieving with a 200-mesh sieve to obtain modified medical stone;
(4) Dissolving 200g of gamma-polyglutamic acid in 2000mL of deionized water to obtain a gamma-polyglutamic acid solution, mixing the gamma-polyglutamic acid solution with the sodium carboxymethylcellulose solution obtained in the step (1), adding 120g of ethylene glycol diglycidyl ether and the modified medical stone obtained in the step (3), crosslinking at 50 ℃ for 36 hours, washing, freezing and drying after reaction for later use;
(5) Grinding the product obtained in the step (4) into powder, then adding the powder into the seaweed essence diluent obtained in the step (2), and carrying out ultrasonic treatment for 7 hours at 90W and 18kHz to obtain the compound active slow-release liquid fertilizer.
Example 5
A preparation method of a composite active slow-release liquid fertilizer comprises the following steps:
(1) Adding 100g of sodium carboxymethylcellulose into 1200mL of deionized water, and uniformly stirring to obtain a sodium carboxymethylcellulose solution for later use;
(2) Adding 200g of seaweed essence into 3000mL of deionized water, and uniformly stirring to obtain seaweed essence diluent for later use;
(3) Adding 200g of medical stone into 2000mL of 15g/L citric acid solution, stirring at 80 ℃ and 250r/min for 10 hours, washing after reaction, and drying to obtain carboxylated medical stone; mixing the obtained carboxylated medical stone with 0.4g of titanium dioxide, 30g of theasaponin and 20g of kaline, heating to 250 ℃ under the protection of nitrogen, reacting for 12 hours, cooling and crushing after the reaction, and sieving by a 300-mesh sieve to obtain modified medical stone;
(4) Dissolving 300g of gamma-polyglutamic acid in 3000mL of deionized water to obtain a gamma-polyglutamic acid solution, mixing the gamma-polyglutamic acid solution with the sodium hydroxymethyl cellulose solution obtained in the step (1), adding 150g of ethylene glycol diglycidyl ether and the modified medical stone obtained in the step (3), crosslinking for 48 hours at 60 ℃, and washing, freezing and drying after reaction for later use;
(5) Grinding the product obtained in the step (4) into powder, then adding the powder into the seaweed essence diluent obtained in the step (2), and carrying out ultrasonic treatment for 8 hours at 100W and 20kHz to obtain the compound active slow-release liquid fertilizer.
Comparative example 1
A preparation method of a liquid fertilizer comprises the following steps:
(1) Adding 50g of sodium carboxymethylcellulose into 500mL of deionized water, and uniformly stirring to obtain a sodium carboxymethylcellulose solution for later use;
(2) Adding 100g of seaweed essence into 2000mL of deionized water, and uniformly stirring to obtain seaweed essence diluent for later use;
(3) Dissolving 200g of gamma-polyglutamic acid in 2000mL of deionized water to obtain a gamma-polyglutamic acid solution, mixing the gamma-polyglutamic acid solution with the sodium carboxymethylcellulose solution obtained in the step (1), adding 50g of ethylene glycol diglycidyl ether, 150g of 200-mesh medical stone, 10g of theasaponin and 10g of kaline, crosslinking for 36 hours at 30 ℃, washing, freezing and drying after reaction for later use;
(4) Grinding the product obtained in the step (3) into powder, then adding the powder into the seaweed essence diluent obtained in the step (2), and carrying out ultrasonic treatment for 5 hours at 60W and 17kHz to obtain the liquid fertilizer.
Comparative example 2
A preparation method of a liquid fertilizer comprises the following steps:
(1) Adding 50g of sodium carboxymethylcellulose into 500mL of deionized water, and uniformly stirring to obtain a sodium carboxymethylcellulose solution for later use;
(2) Adding 100g of seaweed essence into 2000mL of deionized water, and uniformly stirring to obtain seaweed essence diluent for later use;
(3) Adding 150g of medical stone into 1000mL of 10g/L citric acid solution, stirring at 60 ℃ and the rotation speed of 200r/min for 5 hours, washing after reaction, and drying to obtain carboxylated medical stone; mixing the obtained carboxylated medical stone with 0.1g of titanium dioxide, 10g of theasaponin and 10g of kaline, heating to 200 ℃ under the protection of nitrogen, reacting for 8 hours, cooling and crushing after the reaction, and sieving with a 200-mesh sieve to obtain modified medical stone;
(4) And (3) adding the modified medical stone obtained in the step (3) into the seaweed essence diluent obtained in the step (2), mixing with the sodium carboxymethyl cellulose solution obtained in the step (1), and carrying out ultrasonic treatment on the mixture for 5 hours at 60W and 17kHz to obtain the liquid fertilizer.
The liquid fertilizers prepared in examples 1 to 5 and comparative examples 1 to 2 were diluted 300 times to be used as experimental liquid fertilizers. The specific implementation mode is that the same field is divided into 7 areas, and experimental liquid fertilizer is sprayed to the roots of plants every 15 days from the field planting of the peppers to the ripening of the peppers, wherein 5 areas are respectively sprayed to the roots of the plants with the composite active slow-release liquid fertilizer prepared in the embodiments 1-5 of the invention, 2 comparison areas are sprayed with the liquid fertilizer prepared in the comparative examples 1-2, and the application amount of the liquid fertilizer in the 7 areas is 60 kg/mu; the experimental group and the comparison group apply compound fertilizer as base fertilizer according to the dosage of 50 kg/mu in the land preparation stage, and the other field management is the same; the specific experimental data are shown in table 1, wherein the pest damage rate of the peppers in the plot is measured after the peppers are fixedly planted for 15, 30 and 60 days respectively, and the pest damage rate is the ratio of the number of the plants with diseases to the total number of the plants aiming at aphids, cotton bollworms and trialeurodes vaporariorum which are the most common pests of the peppers; the yield increase value was calculated based on the yield of the field area corresponding to comparative example 1.
TABLE 1 statistics of field experimental results for capsicum annuum
The pepper in the test field applied with the liquid fertilizer provided by the invention has good growth vigor, low pest incidence rate, long duration of pest killing effect and obvious effect on pepper yield increase.
Selecting two areas corresponding to the embodiment 1 and the comparative example 2 as soil heavy metal improvement experimental areas, respectively measuring the contents of mercury, cadmium and lead in the soil of the two areas before pepper planting, and measuring the contents of mercury, cadmium and lead in the soil again after the pepper is planted for 30 days.
The mercury content in the soil is measured according to GB/T17136.1997; the content of cadmium and lead in the soil is measured according to GB/T23739-2009, and the specific data are shown in Table 2.
TABLE 2 variation of heavy metal content in soil
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
4. the compound active slow-release liquid fertilizer as claimed in claim 1, wherein the preparation method of the seaweed essence diluent is as follows: mixing refined seaweed and deionized water according to the proportion of 1: mixing evenly 10-20 weight ratio to obtain the seaweed essence diluent.
5. The compound active slow-release liquid fertilizer as claimed in claim 1, wherein the preparation method of the sodium carboxymethyl cellulose solution is as follows: mixing sodium carboxymethylcellulose and deionized water according to the weight ratio of 1: uniformly mixing 8-15 weight percent to obtain the sodium carboxymethyl cellulose solution.
6. A preparation method of the compound active slow-release liquid fertilizer as claimed in any one of claims 1 to 5, characterized by comprising the following steps:
(1) Adding medical stone into citric acid solution, washing and drying after reaction to obtain carboxylated medical stone;
(2) Mixing the carboxylated medical stone obtained in the step (1) with titanium dioxide, theasaponin and kaline, cooling and crushing after reaction, and sieving with a 200-300-mesh sieve to obtain modified medical stone;
(3) Dissolving gamma-polyglutamic acid in deionized water to obtain a gamma-polyglutamic acid solution, mixing the gamma-polyglutamic acid solution with a sodium carboxymethylcellulose solution, adding ethylene glycol diglycidyl ether and the modified medical stone obtained in the step (2), and washing, freezing and drying after reaction for later use;
(4) And (4) grinding the product obtained in the step (3) into powder, then adding the powder into the seaweed essence diluent, and carrying out ultrasonic treatment to obtain the composite active slow-release liquid fertilizer.
7. The preparation method of the compound active slow-release liquid fertilizer as claimed in claim 6, wherein in the step (1), the mass fraction of the citric acid solution is 10-20 g/L; the reaction condition is that the mixture is stirred for 5 to 10 hours at the temperature of between 60 and 90 ℃ and the rotating speed is between 200 and 300r/min.
8. The preparation method of the compound active slow-release liquid fertilizer as claimed in claim 6, wherein in the step (2), the reaction condition is heating to 200-250 ℃ under the protection of nitrogen, and the reaction time is 8-12 h.
9. The preparation method of the compound active slow-release liquid fertilizer as claimed in claim 6, wherein in the step (3), the reaction condition is crosslinking for 36-48 h at 30-60 ℃.
10. The preparation method of the compound active slow-release liquid fertilizer as claimed in claim 6, wherein in the step (4), the ultrasonic power is 60-100W, the frequency is 17-22 kHz, and the ultrasonic treatment is carried out for 5-8 h.
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CN116217298A (en) * | 2022-12-13 | 2023-06-06 | 上饶师范学院 | Modified tea saponin foliar fertilizer auxiliary agent |
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CN107721658A (en) * | 2017-11-25 | 2018-02-23 | 陈琼燕 | A kind of fertilizer synergistic conditioning agent and its production method |
CN112830856A (en) * | 2021-03-03 | 2021-05-25 | 中仓生态农业有限公司 | Preparation method and application of fertilizer synergist |
CN113956094A (en) * | 2021-11-12 | 2022-01-21 | 曲阜师范大学 | Slow-release compound seaweed fertilizer containing garlic extract |
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CN107721658A (en) * | 2017-11-25 | 2018-02-23 | 陈琼燕 | A kind of fertilizer synergistic conditioning agent and its production method |
CN112830856A (en) * | 2021-03-03 | 2021-05-25 | 中仓生态农业有限公司 | Preparation method and application of fertilizer synergist |
CN113956094A (en) * | 2021-11-12 | 2022-01-21 | 曲阜师范大学 | Slow-release compound seaweed fertilizer containing garlic extract |
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