CN112745167B - Amino acid water-soluble fertilizer containing chitosan oligosaccharide and preparation method thereof - Google Patents
Amino acid water-soluble fertilizer containing chitosan oligosaccharide and preparation method thereof Download PDFInfo
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- CN112745167B CN112745167B CN202110213888.7A CN202110213888A CN112745167B CN 112745167 B CN112745167 B CN 112745167B CN 202110213888 A CN202110213888 A CN 202110213888A CN 112745167 B CN112745167 B CN 112745167B
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C5/00—Fertilisers containing other nitrates
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G5/00—Fertilisers characterised by their form
- C05G5/20—Liquid fertilisers
- C05G5/23—Solutions
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Abstract
The invention discloses a chitosan oligosaccharide-containing amino acid water-soluble fertilizer which is prepared from the following raw materials in parts by weight: 38-40 parts of pure water, 0.5-1 part of N-acetylthioproline, 2-3 parts of glycine, 1-4 parts of sorbitol, 17-20 parts of calcium nitrate tetrahydrate, 1-2 parts of magnesium nitrate hexahydrate, 28-30 parts of composite amino acid powder, 5 parts of chitosan oligosaccharide, 0.1-0.5 part of thickening agent and 1-3 parts of pH regulator; the preparation method of the water soluble fertilizer comprises the following steps: 1) Adding pure water into a reaction kettle, starting a stirrer, adding N-acetylthioproline, glycine and sorbitol, and stirring until the pure water is completely dissolved; 2) Adding calcium nitrate tetrahydrate and magnesium nitrate hexahydrate, and stirring until the calcium nitrate tetrahydrate and the magnesium nitrate hexahydrate are completely dissolved; 3) Adding composite amino acid powder and chitosan oligosaccharide, and stirring until the mixture is completely dissolved; 4) Adding a thickening agent, and stirring until the thickening agent is completely dissolved; 5) Standing to normal temperature, adding a pH regulator to adjust the pH to 5.0-7.0, and performing spot inspection to obtain the product. The water-soluble fertilizer prepared by the invention contains 5% of chitosan oligosaccharide, has stable properties and obvious fertilizer efficiency, and can be mixed with part of suspending agent for use.
Description
Technical Field
The invention relates to the field of liquid fertilizers, in particular to a chitosan oligosaccharide-containing amino acid water-soluble fertilizer and a preparation method thereof.
Background
The research on liquid fertilizers in China is late, the initial products of the liquid fertilizers are mostly elemental fertilizers such as ammonia water, urea ammonium nitrate liquid, nitric acid and phosphoric acid, the fertilizers are mostly elemental fertilizers, and are mostly strong acid and strong alkaline fertilizers, and the liquid fertilizers are very inconvenient to use. With the improvement of the technology, a plurality of functional fertilizers appear on the market, the functions of the fertilizers are that the biological stimulin components such as amino acid, humic acid, alginic acid and the like are added on the basis of common large and medium trace element fertilizers such as nitrogen, phosphorus, potassium, calcium, magnesium, iron, manganese, zinc, copper, molybdenum and the like, and the formed fertilizers not only have the nutrition function, but also have the functions of regulating and controlling nutrition absorption, stimulating the physiology and biochemistry of crops, resisting plant diseases and insect pests and the like.
The area of 71 percent of the earth is ocean, the ocean has abundant biological resources, at least 25 thousands of organisms, more than 2 thousands of crustaceans, and the outer surface shells of the crustaceans are often used as byproducts of other industries and are wasted. With the improvement of the technology, the technology for extracting chitin, chitosan and chitosan oligosaccharide from the outer surface shell of crustacean is mature day by day, for example, in the prior art, the chitin can be obtained by taking shrimp and crab shells and other substances as raw materials and decalcifying and protein, but is not easy to be absorbed, chitosan can be obtained after deacetylation, and chitosan oligosaccharide can be obtained after further enzymolysis. Common chitosan oligosaccharide is divided into liquid and solid, and the chitosan oligosaccharide contains rich C, N which can be used as nutrient for plant growth, not only has the functions of killing virus, bacteria and fungi, but also has the effects of nutrition, regulation, detoxification and antibiosis, so that the chitosan oligosaccharide is widely used as pesticide and fertilizer in agriculture. The chitosan oligosaccharide is also called oligomeric chitosan, amino-oligosaccharin and chitooligosaccharide, and is water-soluble oligomeric glucosamine with low molecular weight and the polymerization degree of 2-10, which is connected by beta-1,4 glycosidic bond, and the chitosan oligosaccharide is divided into food-grade chitosan oligosaccharide, agricultural-grade chitosan oligosaccharide and feed-grade chitosan oligosaccharide according to the application field, the agricultural-grade chitosan oligosaccharide is divided into amino-oligosaccharin and chitooligosaccharide 2, wherein the amino-oligosaccharin with the molecular weight of 340-2500 Da is called amino-oligosaccharin applied to biological pesticide, and belongs to the field of pesticide; the chitosan oligosaccharide (also called chitosan oligosaccharide) with molecular weight of 340-6000 Da, called biostimulant, requires polymerization degree of 2-30.
The patent of taking amino-oligosaccharide as biological pesticide is introduced more, for example, CN 110915653B provides the method that 2-8 mg/L amino-oligosaccharide can be utilized to improve the induction efficiency of fir somatic embryo; CN 106508911B, CN 106693931B, CN 105707081B, CN 106234369B, CN 106035334B and the like all provide methods for improving the pesticide effect by combining amino oligosaccharide and other pesticide components. The technology of adding amino-oligosaccharin into fertilizer has been disclosed as pesticide, for example, CN 104276891B provides a microelement type foliar fertilizer containing 0.5-0.8% of amino-oligosaccharin, and the embodiment shows that the foliar fertilizer of amino-oligosaccharin has the effects of promoting the increase of diameter and diameter section of sugarcane and promoting the yield increase of sugarcane; the invention patent with application number 201910701841.8 provides a functional coated slow release fertilizer containing 4-7 parts of amino-oligosaccharin, and the embodiment shows that the amino-oligosaccharin can improve the yield of rice and promote the plump rice grains. However, as a fertilizer product containing amino-oligosaccharin, the amino-oligosaccharin, which is a pesticide component, is contained in the fertilizer product, and can be popularized as a pesticide product for acquiring pesticide operation rights, and if the amino-oligosaccharin is used as a fertilizer product, the popularization is illegal.
The plant protection and flying prevention technology is taken as an effective tool for the development of new agriculture in a new era, the plant protection and flying prevention requires that pesticide and fertilizer can be mixed for use, but the pesticide and fertilizer are usually mixed for use to a limited extent due to the self physical and chemical properties of the pesticide and the fertilizer, the compatibility of the pesticide and the fertilizer is influenced, and particularly when the fertilizer and a suspending agent are mixed for use, the suspending rate of the suspending agent is seriously influenced by the fertilizer, so that the fertilizer is precipitated in a fertilizing container, a fertilizing machine is blocked, and the pesticide effect is influenced. When most of chitosan oligosaccharide products on the market, no matter pesticides and fertilizer products, contain a certain amount of chitosan oligosaccharide and are mixed with a common suspending agent for use, more precipitates are generated within 30 minutes, the drug effect and the fertilizer effect of the chitosan oligosaccharide and the suspending agent are seriously influenced, a spray head is blocked, and the agricultural material loss is caused. CN 103210922B, CN 104522004B and 'formulation development of 22% amino-oligosaccharin and fenoxanil SC' directly compound amino-oligosaccharin and pesticide to form a suspending agent pesticide product containing the amino-oligosaccharin, wherein the suspending agent pesticide product has a pesticide effect function, but the fertilizer effect function is not reflected yet, and the prior art has no report that chitosan oligosaccharide can be prepared into a fertilizer product and is mixed with part of a suspending agent for use.
In conclusion, in the current research and published patent, no legal fertilizer product containing the chitosan oligosaccharide and capable of being mixed with the suspending agent is available.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a legal chitosan-containing amino acid fertilizer product which can be mixed with a suspending agent for use. The invention relates to an amino acid fertilizer product containing chitosan oligosaccharide, which adopts N-acetylthioproline glycine and sorbitol to chelate calcium and magnesium, achieves stable product system by adjusting acid-base and solution viscosity, has simple production process and low product cost, and is suitable for the production of various legal enterprises.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
the amino acid water-soluble fertilizer containing chitosan oligosaccharide comprises the following raw materials in parts by weight: 38-40 parts of pure water, 0.5-1 part of N-acetylthioproline, 2-3 parts of glycine, 1-4 parts of sorbitol, 17-20 parts of calcium nitrate tetrahydrate, 1-2 parts of magnesium nitrate hexahydrate, 28-30 parts of composite amino acid powder, 5 parts of chitosan oligosaccharide, 0.1-0.5 part of thickening agent and 1-3 parts of pH regulator.
Furthermore, the chitosan oligosaccharide is one of chitosan oligosaccharides, the molecular weight of the chitosan oligosaccharide is 2500-6000Da, and the chitosan oligosaccharide meets the detection requirements of T/CAI 002-2018 biostimulant chitosan oligosaccharide.
Further, the thickening agent is xanthan gum or sodium carboxymethyl cellulose.
Further, the pH regulator is one or two of acetic acid and ethanolamine.
Further, the preparation method of the chitosan oligosaccharide-containing amino acid water-soluble fertilizer comprises the following steps:
1) According to the measurement, adding pure water into a reaction kettle, starting a stirrer, controlling the temperature to be 60 ℃, adding N-acetylthioproline, glycine and sorbitol, and stirring for 10 minutes until all the N-acetylthioproline, the glycine and the sorbitol are dissolved;
2) According to the measurement, calcium nitrate tetrahydrate and magnesium nitrate hexahydrate are added and stirred for 30 minutes until the calcium nitrate tetrahydrate and the magnesium nitrate hexahydrate are completely dissolved;
3) Adding the composite amino acid powder and the chitosan oligosaccharide according to the amount, and stirring for 30 minutes until the mixture is completely dissolved;
4) Adding the thickening agent according to the measurement, and stirring for 2 hours until the thickening agent is completely dissolved;
5) According to the measurement, the materials in the reaction kettle are kept stand for 6 hours to normal temperature, a pH regulator is added to adjust the pH of the product to 5.0-7.0, and the qualified product can be obtained by sampling inspection.
Compared with the prior art, the invention has the beneficial effects that:
(1) The chitosan oligosaccharide fertilizer product prepared by the invention does not contain pesticide components and is a legally sold fertilizer product.
(2) The chitosan-containing amino acid water-soluble fertilizer prepared by the invention has good stability, and has no precipitation, flocculation and flatulence after being refrigerated for 7 days at 0 ℃ and stored for 14 days at 54 ℃.
(3) The water-soluble fertilizer containing 5% of chitosan oligosaccharide amino acid prepared by the invention can be mixed with a suspending agent for use, and is suitable for various occasions where medicinal fertilizers are applied simultaneously.
(4) The product of the invention has the advantages of legal compliance and obvious fertilizer effect, the technical indexes of the product completely conform to the standards of NY1429-2010 amino acid-containing water-soluble fertilizer products, the product has conventional medium elements, functional substances of amino acid and chitosan oligosaccharide, and can stimulate the physiology and biochemistry of crops and improve the disease resistance of the crops in addition to maintaining the nutrition required by the plants, thereby achieving the purposes of increasing the yield and gaining the harvest.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A preparation method of chitosan oligosaccharide-containing amino acid water-soluble fertilizer comprises the following steps:
1) According to the measurement, 40 parts of pure water is added into a reaction kettle, a stirrer is started, the temperature is controlled to be 60 ℃, 0.5 part of N-acetylthioproline, 3 parts of glycine and 2.4 parts of sorbitol are added and stirred for 10 minutes until the pure water is completely dissolved;
2) According to the measurement, 17 parts of calcium nitrate tetrahydrate and 2 parts of magnesium nitrate hexahydrate are added, and stirred for 30 minutes until the calcium nitrate tetrahydrate and the magnesium nitrate hexahydrate are completely dissolved;
3) Adding 28 parts of composite amino acid powder and 5 parts of chitosan oligosaccharide with the molecular weight of 2500Da according to the weight, and stirring for 30 minutes until the chitosan oligosaccharide is completely dissolved;
4) Adding 0.1 part of xanthan gum according to the measurement, and stirring for 2 hours until the xanthan gum is completely dissolved;
5) According to the measurement, the materials in the reaction kettle are kept stand for 6 hours to normal temperature, 1 part of acetic acid and 1 part of ethanolamine are added to adjust the pH value of the product to 6.47, and the qualified product can be obtained through sampling inspection.
Example 2
A preparation method of chitosan oligosaccharide-containing amino acid water-soluble fertilizer comprises the following steps:
1) Adding 38 parts of pure water into a reaction kettle according to the measurement, starting a stirrer, controlling the temperature to be 60 ℃, adding 1 part of N-acetylthioproline, 2 parts of glycine and 1 part of sorbitol, and stirring for 10 minutes until all the N-acetylthioproline, the glycine and the sorbitol are dissolved;
2) According to the measurement, 20 parts of calcium nitrate tetrahydrate and 1.5 parts of magnesium nitrate hexahydrate are added and stirred for 30 minutes until the calcium nitrate tetrahydrate and the magnesium nitrate hexahydrate are completely dissolved;
3) Adding 30 parts of compound amino acid powder and 5 parts of chitosan oligosaccharide with the molecular weight of 3000Da according to the measurement, and stirring for 30 minutes until the chitosan oligosaccharide is completely dissolved;
4) According to the measurement, 0.5 part of sodium carboxymethyl cellulose is added and stirred for 2 hours until the sodium carboxymethyl cellulose is completely dissolved;
5) According to the measurement, the materials in the reaction kettle are kept stand for 6 hours to normal temperature, 1 part of acetic acid is added to adjust the pH value of the product to 5.88, and the qualified product can be obtained by sampling inspection.
Example 3
A preparation method of chitosan oligosaccharide-containing amino acid water-soluble fertilizer comprises the following steps:
1) Adding 38 parts of pure water into a reaction kettle according to the measurement, starting a stirrer, controlling the temperature to be 60 ℃, adding 0.7 part of N-acetylthioproline, 2 parts of glycine and 4 parts of sorbitol, and stirring for 10 minutes until all the N-acetylthioproline, the glycine and the sorbitol are dissolved;
2) According to the measurement, 18 parts of calcium nitrate tetrahydrate and 1 part of magnesium nitrate hexahydrate are added, and the mixture is stirred for 30 minutes until the calcium nitrate tetrahydrate and the magnesium nitrate hexahydrate are completely dissolved;
3) Adding 28 parts of compound amino acid powder and 5 parts of chitosan oligosaccharide with the molecular weight of 6000Da according to the weight, and stirring for 30 minutes until the chitosan oligosaccharide is completely dissolved;
4) Adding 0.3 part of xanthan gum according to the measurement, and stirring for 2 hours until the xanthan gum is completely dissolved;
5) According to the measurement, the materials in the reaction kettle are kept stand for 6 hours to normal temperature, 1 part of acetic acid and 2 parts of ethanolamine are added to adjust the pH value of the product to 6.63, and the qualified product can be obtained through sampling inspection.
Example 4
A preparation method of chitosan oligosaccharide-containing amino acid water-soluble fertilizer comprises the following steps:
1) According to the measurement, 38.5 parts of pure water is added into a reaction kettle, a stirrer is started, the temperature is controlled to be 60 ℃, 0.5 part of N-acetylthioproline, 2.5 parts of glycine and 2 parts of sorbitol are added and stirred for 10 minutes until the pure water is completely dissolved;
2) According to the measurement, 19 parts of calcium nitrate tetrahydrate and 2 parts of magnesium nitrate hexahydrate are added, and stirred for 30 minutes until the calcium nitrate tetrahydrate and the magnesium nitrate hexahydrate are completely dissolved;
3) Adding 28.5 parts of composite amino acid powder and 5 parts of chitosan oligosaccharide with the molecular weight of 4500Da according to the weight, and stirring for 30 minutes until the chitosan oligosaccharide is completely dissolved;
4) According to the measurement, 0.5 part of sodium carboxymethyl cellulose is added and stirred for 2 hours until the sodium carboxymethyl cellulose is completely dissolved;
5) According to the measurement, the materials in the reaction kettle are kept stand for 6 hours to normal temperature, 0.75 part of acetic acid and 0.75 part of ethanolamine are added to adjust the pH value of the product to 6.10, and the qualified product can be obtained through sampling inspection.
The products prepared in the above examples 1-4 are subjected to spot inspection, the detection results all reach the NY1429-2010 amino acid-containing water-soluble fertilizer product standard, the products contain 5% of chitosan oligosaccharide (the density is not less than 1.25g/ml, the chitosan oligosaccharide content is not less than 62 g/L), the molecular weight of the 5% of chitosan oligosaccharide in the products is controlled to be 2500-6000Da, the detection requirements of T/CAI 002-2018 biostimulan chitosan oligosaccharide are met, the products can be legally used and popularized in fertilizer products, and the specific detection results are shown in Table 1:
table 1 results of examination of products prepared in examples 1 to 4
For the products prepared in examples 1-4 above, the product was prepared according to the examples and 45% pyrazole tebuconazole suspending agent (pyraclostrobin 15%, tebuconazole 30%) =1:1,1:2,2:1, and example product and 240g/L thifluzamide suspension =1:1,1:2,2:1, determining the suspension rate in standard hard water according to a GB/T14285-2006 pesticide suspension rate determination method, selecting a 5% amino-oligosaccharin product on the market as a reference, and specifically determining results as shown in Table 2:
TABLE 2 suspension percentage of the products prepared in examples 1-4 when used in combination with 45% pyrazole tebuconazole suspension or 240g/L thifluzamide suspension
As can be seen from the data in Table 2, the products prepared in examples 1-4 of the present invention were mixed with either 45% pyrazole tebuconazole suspension or 240g/L thifluzamide suspension in a ratio of 1:1,1:2,2:1, the suspension rates of the 45% pyrazole-tebuconazole suspending agent and the 240g/L thifluzamide suspending agent are not affected, while the suspension rates of the 45% pyrazole-tebuconazole suspending agent and the 240g/L thifluzamide suspending agent are seriously affected by the 5% amino-oligosaccharin product in the control group, the precipitation of the suspending agent is also caused, the spray head is easily blocked, the pesticide and fertilizer effect is reduced, and the economic loss is easily caused. It can be seen that the products prepared in examples 1 to 4 of the present invention can be used in combination with 45% pyrazole-tebuconazole suspension or 240g/L thifluzamide suspension, and can be applied to various agricultural techniques and agricultural machinery for fertilization and application.
The products prepared in examples 1 to 4 were subjected to potting experiments with fertilizer efficiency, 20 leaf lettuce big tips were used in each group of 6 pots, and 20 leaf lettuce seedlings were planted in each pot, and germination rate was measured, thinning was performed after 3 true leaves grew out of the lettuce seedlings, and 3 leaf lettuce seedlings were retained, using coconut husk, vermiculite, perlite as the substrate, and the ratio was 5:1:1. the first group of products prepared according to example 1 and the second group of products prepared according to example 2The third group uses the product prepared in example 3, the fourth group uses the product prepared in example 4, the fifth group is a blank group and sprays pure water with the same amount, the sixth group uses a common water-soluble fertilizer containing amino acid (the index is that the content of free amino acid is more than or equal to 100g/L, calcium and magnesium are more than or equal to 30g/L, wherein, calcium is more than or equal to 25g/L, and magnesium is more than or equal to 5 g/L) in the control group, and the six groups of experiments adopt 1000 times of foliage spraying to carry out the foliage spraying, and each time is 7 days; the nutrient indexes of the six groups of root-irrigation fertilizers are N17 percent and P 2 O 5 17％，K 2 O17%, B0.1%, zn 0.4%, diluting 1000 times, irrigating the root once every 3 days, irrigating the root 50ml each time, simultaneously irrigating 50ml, the whole lettuce growth cycle is 45 days, spraying on the leaf surface 6 times in total, irrigating the root 15 times, measuring the height and weight of each plant seedling to the harvest time, and converting the yield according to 20000 plants per mu of lettuce seedlings, wherein the concrete test data are shown in Table 3:
TABLE 3 leaf lettuce test data
As shown by data in Table 3, the fertilizers prepared in examples 1-4 of the invention have no influence on germination percentage, which indicates that the products prepared in examples 1-4 are safe, compared with common amino acid water-soluble fertilizers in the market, the fertilizers prepared in examples 1-4 have a promoting effect on the growth of leaf lettuce, and the fertilizers prepared in examples 1-4 increase the yield of leaf lettuce by 3.41-8.73%, so that the yield of leaf lettuce can be obviously improved.
Claims (1)
1. The amino acid water-soluble fertilizer containing chitosan oligosaccharide is characterized by comprising the following raw materials in parts by weight: 38-40 parts of pure water, 0.5-1 part of N-acetylthioproline, 2-3 parts of glycine, 1-4 parts of sorbitol, 17-20 parts of calcium nitrate tetrahydrate, 1-2 parts of magnesium nitrate hexahydrate, 28-30 parts of composite amino acid powder, 5 parts of chitosan oligosaccharide, 0.1-0.5 part of thickening agent and 1-3 parts of pH regulator;
the molecular weight of the chitosan oligosaccharide is 2500-6000Da;
the thickening agent is xanthan gum or sodium carboxymethyl cellulose;
the pH regulator is one or two of acetic acid and ethanolamine;
the preparation method of the chitosan oligosaccharide-containing amino acid water-soluble fertilizer comprises the following steps:
1) According to the measurement, adding pure water into a reaction kettle, starting a stirrer, controlling the temperature to be 60 ℃, adding N-acetylthioproline, glycine and sorbitol, and stirring for 10 minutes until all the N-acetylthioproline, the glycine and the sorbitol are dissolved;
2) According to the measurement, adding calcium nitrate tetrahydrate and magnesium nitrate hexahydrate, and stirring for 30 minutes until the calcium nitrate tetrahydrate and the magnesium nitrate hexahydrate are completely dissolved;
3) Adding the composite amino acid powder and the chitosan oligosaccharide according to the amount, and stirring for 30 minutes until the mixture is completely dissolved;
4) Adding the thickening agent according to the measurement, and stirring for 2 hours until the thickening agent is completely dissolved;
5) According to the measurement, the materials in the reaction kettle are kept stand for 6 hours to normal temperature, a pH regulator is added to adjust the pH of the product to 5.0-7.0, and the qualified product can be obtained by sampling inspection.
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| CN106316585A (en) * | 2016-08-12 | 2017-01-11 | 董向波 | Preparation method of biostimulant medium element water-soluble fertilizer |
| CN111763115B (en) * | 2020-07-08 | 2022-06-10 | 郑州郑氏化工产品有限公司 | Fertilizer synergist and preparation method and application thereof |
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