CN106800472B - Composite modified polyurethane coating liquid, controlled-release fertilizer and preparation method thereof - Google Patents
Composite modified polyurethane coating liquid, controlled-release fertilizer and preparation method thereof Download PDFInfo
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- CN106800472B CN106800472B CN201710131918.3A CN201710131918A CN106800472B CN 106800472 B CN106800472 B CN 106800472B CN 201710131918 A CN201710131918 A CN 201710131918A CN 106800472 B CN106800472 B CN 106800472B
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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
- C05G5/30—Layered or coated, e.g. dust-preventing coatings
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B7/00—Fertilisers based essentially on alkali or ammonium orthophosphates
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C1/00—Ammonium nitrate fertilisers
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Abstract
The invention discloses a composite modified polyurethane coating liquid, a controlled release fertilizer and a preparation method thereof, wherein the preparation method of the polyurethane coating controlled release fertilizer comprises the following steps: (1) uniformly mixing vegetable oil polyalcohol and attapulgite according to a predetermined proportion to obtain a component A; (2) reacting polymethylene polyphenyl isocyanate with cardanol with the molar ratio of 10-15% for 1-3 hours at the temperature of 70-80 ℃ to obtain a component B; (3) uniformly mixing the A, B components in proportion to obtain a plant oil-based attapulgite hybrid composite modified polyurethane coating solution; (4) preheating the granulated fertilizer to be coated; (5) spraying the composite modified polyurethane coating slurry on the surface of the preheated fertilizer particles; (6) and after the plant oil-based polyurethane coating slurry is cured, repeatedly spraying the plant oil-based polyurethane coating slurry for 3-6 times to obtain the plant oil-based attapulgite hybrid composite modified polyurethane coated controlled release fertilizer.
Description
Technical Field
The invention relates to a coating material, a coated controlled-release fertilizer and a preparation method thereof, in particular to a plant oil-based and attapulgite hybrid composite modified polyurethane coating liquid, a controlled-release fertilizer and a preparation method thereof.
Background
The slow controlled release fertilizer is a novel fertilizer, and is widely concerned in the whole world due to the unique advantages of energy conservation, environmental protection, high fertilizer utilization rate, yield and efficiency increase, labor and time conservation and the like. The slow-release fertilizer mainly has three mechanisms to achieve the purpose of slow release: firstly, adding a nitrogen inhibitor; secondly, adding formaldehyde and urea; and thirdly, coating the fertilizer. The controlled release fertilizer is a high-grade form of the controlled release fertilizer, the coated controlled release fertilizer can control and release all nutrients contained in fertilizer particles, the overall controlled release performance is strong, and the coated controlled release fertilizer is a key novel fertilizer for development and application of the current controlled release fertilizer. China also clearly proposes the industry of rapidly developing the controlled release fertilizer in important documents such as the scheme outline of the eleventh five-year plan for national economy and social development (2006 + 2010), the scheme outline of the eleventh five-year plan for national agriculture and rural economy development (2006 + 2010) of the department of agriculture, and the like, and the controlled release fertilizer is rapidly developed in the near year under the great promotion of China, so that the market space is huge.
The coated controlled release fertilizer is divided from the category of coating materials into inorganic coated controlled release fertilizer and organic coated controlled release fertilizer, wherein the resin coated controlled release fertilizer formed by organic substances is a fine product in the slow controlled release fertilizer. Because the technical content is high, the nutrient release synchronism is precise, the performance is far superior to other slow controlled release fertilizers, but still a plurality of technical difficulties need to be overcome, such as: no solvent, continuous production, low cost of membrane material, biodegradability and the like.
In China, the process of preparing the coated controlled release fertilizer by dissolving high molecular materials such as polyolefin materials and the like by using an organic solvent and then spraying coated fertilizer particles is mature, but has the defects of high production cost, low continuity level, environmental pollution caused by using the organic solvent in the production process, difficult degradation of a film material and the like. Aiming at the requirements of coating materials, green processes, environmental protection and the like, the in-situ polymerization film-forming reaction of polyurethane is more and more a hot point of research; therefore, there is a need to provide a new coated controlled release fertilizer, which has the advantages of wide sources of coated raw materials, low price, easy obtainment, no toxicity, no harm, simple production process and good controlled release effect.
Disclosure of Invention
The invention aims to solve the technical problem of providing a plant oil-based and attapulgite hybrid composite modified polyurethane coating liquid, a controlled release fertilizer and a preparation method thereof.
The technical scheme adopted by the invention for solving the technical problems is to provide a composite modified polyurethane coating liquid, wherein the polyurethane coating liquid is prepared by mixing vegetable oil polyalcohol containing attapulgite and isocyanate modified by cardanol.
The composite modified polyurethane coating liquid comprises a base material and a carrier, wherein the carrier is a cardanol modified isocyanate, the cardanol modified isocyanate is used as a base material, the carrier is a composite modified polyurethane coating liquid, and the molar ratio of hydroxyl groups in the vegetable oil polyalcohol to isocyanate groups in the cardanol modified isocyanate is [ OH ]: [ NCO ]: 1: 0.8-1.2.
The composite modified polyurethane coating liquid is characterized in that the vegetable oil polyol is at least one selected from castor oil polyol, hydrogenated castor oil polyol, soybean oil polyol and hydroxylated rapeseed oil polyol; the isocyanate is selected from one or any combination of the following isocyanates: toluene diisocyanate, diphenylmethane-4, 4 '-diisocyanate, modified diphenylmethane-4, 4' -diisocyanate, polymethylene polyphenyl polyisocyanate.
The composite modified polyurethane coating liquid comprises the following components in parts by mass, wherein the addition amount of the attapulgite is 20-30% of the mass of the vegetable oil; the attapulgite is attapulgite with fineness of more than 400 meshes.
The composite modified polyurethane coating liquid comprises the following components, wherein the isocyanate is polymethylene polyphenyl polyisocyanate, and the mass content of isocyanate groups in the isocyanate is 30.2% -32.0%.
The composite modified polyurethane coating liquid is prepared by adding 10-15% mol ratio of cardanol into polymethylene polyphenyl isocyanate and reacting at 70-80 ℃ for 1-3 hours.
The invention provides a vegetable oil-based polyurethane coated controlled-release fertilizer, which comprises a granulated fertilizer and a polyurethane coated coating coated on the granulated fertilizer, wherein the polyurethane coated coating is prepared from the vegetable oil-based polyurethane coated liquid.
The vegetable oil-based polyurethane coated controlled-release fertilizer is characterized in that the mass of the polyurethane coated coating is 3% -6% of the mass of the granulated fertilizer.
The third technical scheme adopted by the invention for solving the technical problems is to provide a preparation method of the vegetable oil-based polyurethane coated controlled-release fertilizer, which comprises the following steps: (1) uniformly mixing vegetable oil polyalcohol and attapulgite according to a predetermined proportion to obtain a component A; (2) adding cardanol with the molar ratio of 10-15% into polymethylene polyphenyl isocyanate to react for 1-3 hours at the temperature of 70-80 ℃ to obtain a component B; (3) uniformly mixing the A, B components in proportion to obtain a plant oil-based attapulgite hybrid composite modified polyurethane coating solution; (4) preheating the granulated fertilizer to be coated; (5) spraying the composite modified polyurethane coating slurry on the surface of the preheated fertilizer particles; (6) and after the plant oil-based polyurethane coating slurry is cured, repeatedly spraying the plant oil-based polyurethane coating slurry for 3-6 times to obtain the plant oil-based attapulgite hybrid composite modified polyurethane coated controlled release fertilizer.
The preparation method of the vegetable oil-based polyurethane coated controlled-release fertilizer comprises the following steps of preheating the granulated fertilizer in a coating machine; the preheating temperature is 55-75 ℃.
Compared with the prior art, the invention has the following beneficial effects: 1. according to the plant oil-based and attapulgite hybrid composite modified polyurethane coating liquid, the controlled-release fertilizer and the preparation method thereof, the plant oil-based polyol can adopt castor oil and other plant oil containing a large amount of hydroxyl groups, and has the advantages of wide sources, low price, easy obtainment, biodegradability and the like; meanwhile, the organic silicon fertilizer is easy to react with polyisocyanate on the surface of fertilizer particles to form a film, and the film forming process is simple; because the polyurethane resin has the advantages of wear resistance, solvent resistance, high adhesion, excellent mechanical property and the like, the combination of soft and hard segments and the physical and chemical crosslinking in the polyurethane coexist, and after proper process conditions are determined, a good controlled release effect can be achieved. 2. The attapulgite hybridized with the vegetable oil base has wide sources, is cheap and easy to obtain, and is green and environment-friendly. The structure of the coating contains a large amount of hydroxyl, so that the coating cost is effectively reduced, the coating strength with isocyanate can be enhanced, and the stability of the coating structure is greatly improved. Meanwhile, the compatibility of the fertilizer to soil is enhanced, and the fertilizer is easy to absorb and utilize by crops. 3. After the isocyanate for coating is modified by cardanol, the toughness of the whole macromolecular skeleton structure can be effectively improved, and the defects of brittleness, breakage and the like of a coating material are effectively prevented. Meanwhile, the sources of related materials are easy to obtain, the degradation is facilitated, and the negative effects of the coating material on the soil environment after the nutrients of the controlled release fertilizer are released can be effectively eliminated.
Drawings
FIG. 1 is a schematic diagram of a film-forming structure of a composite modified polyurethane coated controlled-release fertilizer in an embodiment of the invention.
Detailed Description
The invention is further described below with reference to the figures and examples.
The invention provides a plant oil-based attapulgite hybrid composite modified polyurethane coating solution which is prepared by mixing vegetable oil polyalcohol containing attapulgite and cardanol modified isocyanate. The molar ratio of hydroxyl groups in the vegetable oil polyalcohol to isocyanate groups in the cardanol modified isocyanate is [ OH ]: 1: 0.8-1.2. The vegetable oil polyol is selected from at least one of castor oil polyol, hydrogenated castor oil polyol, soybean oil polyol and hydroxylated rapeseed oil polyol. Preferably, the vegetable oil polyol is a castor oil polyol.
The addition amount of the attapulgite is 20-30% of the mass of the vegetable oil, and in order to achieve the effect of uniform dispersion, the attapulgite with the fineness of over 400 meshes is commercially available.
The isocyanate is selected from one or any combination of the following isocyanates: toluene diisocyanate, diphenylmethane-4, 4 '-diisocyanate, modified diphenylmethane-4, 4' -diisocyanate, polymethylene polyphenyl polyisocyanate. Further preferable is polymethylene polyphenyl polyisocyanate, and the mass content of isocyanate groups in the isocyanate is 30.2-32.0%.
The cardanol modified polyisocyanate is prepared by reacting polymethylene polyphenyl isocyanate with cardanol with the molar ratio of 10% -15% at 70-80 ℃ for 2 hours. Possible equations are as follows:
the plant oil-based attapulgite hybrid composite modified polyurethane coated controlled-release fertilizer provided by the invention comprises a granular fertilizer and a polyurethane coated coating coated on the granular fertilizer, wherein the polyurethane coated coating is the plant oil-based attapulgite hybrid composite modified polyurethane film. The mass of the polyurethane coating is 3-6% of the mass of the granular fertilizer. The particle size of the granular fertilizer is in the range of 2.00mm-4.75mm, and the granular fertilizer contains at least one of the following nutrients: nitrogen, phosphorus, potassium, calcium, magnesium, sulfur and trace elements; the fertilizer is a granular fertilizer such as compound fertilizer, urea, potassium sulfate, ammonium sulfate, potassium nitrate, ammonium dihydrogen phosphate or diammonium hydrogen phosphate.
The following is a specific description of the preparation method of the plant oil-based attapulgite hybrid composite modified polyurethane coated controlled-release fertilizer, and the present invention is not limited to the following examples, which are all conventional methods unless otherwise specified, and the materials are all commercially available, and the fertilizer particles used are selected from NPK composite fertilizer particles, urea, potassium sulfate, ammonium sulfate, potassium nitrate, ammonium dihydrogen phosphate, diammonium hydrogen carbonate, and other granular fertilizers.
Example 1
(1) 24.50g of castor oil and 7.00g of attapulgite are weighed in advance, added into a small beaker and uniformly mixed by a magnetic stirrer to obtain the component A. (2) Weighing 16.60g of polymethylene polyphenyl polyisocyanate and 3.80g of cardanol in advance, heating to 75 ℃, and reacting for 2 hours to obtain the cardanol modified polymethylene polyphenyl polyisocyanate and obtain the component B. (3) Evenly mixing the A, B components to obtain a plant oil-based attapulgite hybrid composite modified polyurethane coating solution; (4) weighing 1000g of 15-15-15 compound fertilizer particles with the particle size of 2.00-4.75 mm, placing the 15-15-15 compound fertilizer particles in a film coating machine, and starting the film coating machine to preheat the fertilizer particles until the temperature of the fertilizer particles reaches 70 ℃; (5) spraying the plant oil-based attapulgite hybrid composite modified polyurethane coating slurry prepared in the step (3) on the surface of the 15-15-15 compound fertilizer particles preheated in the step (4), continuing heating and heat preservation for in-situ polymerization reaction, and curing for 5-6 minutes; (6) the input amount of the coating material is 1 percent of the total weight of the granulated fertilizer each time, the above 5 times are repeated, and the temperature is cooled to be below 40 ℃, so that the plant oil-based attapulgite hybrid composite modified polyurethane coated controlled release fertilizer with the coating amount of 5 percent is obtained.
The controlled release performance of the prepared coated controlled release fertilizer is measured by HG/T4215-.
Example 2
(1) Weighing 18.40g of castor oil and 5.50g of attapulgite in advance, adding into a small beaker, and uniformly mixing by a magnetic stirrer to obtain the component A. (2) Weighing 8.10g of polymethylene polyphenyl polyisocyanate and 1.54g of cardanol in advance, heating to 78 ℃, and reacting for 2 hours to obtain the cardanol modified polymethylene polyphenyl polyisocyanate and obtain the component B. (3) Evenly mixing the A, B components to obtain a plant oil-based attapulgite hybrid composite modified polyurethane coating solution; (4) weighing 1000g of 15-15-15 compound fertilizer particles with the particle size of 2.00-4.75 mm, placing the 15-15-15 compound fertilizer particles in a film coating machine, and starting the film coating machine to preheat the fertilizer particles until the temperature of the fertilizer particles reaches 65 ℃; (5) spraying the plant oil-based attapulgite hybrid composite modified polyurethane coating slurry prepared in the step (3) on the surface of the 15-15-15 compound fertilizer particles preheated in the step (4), continuing heating and heat preservation for in-situ polymerization reaction, and curing for 5-6 minutes; (6) the input amount of the coating material is 1 percent of the total weight of the granulated fertilizer each time, the above steps are repeated for 3 times, and the temperature is cooled to be below 40 ℃, so that the plant oil-based attapulgite hybrid composite modified polyurethane coated controlled release fertilizer with the coating amount of 3 percent is obtained.
The controlled release performance of the prepared coated controlled release fertilizer is measured by HG/T4215-2011 standard, the release period is 60 days, the initial nutrient release rate is 1.53 percent, the 28-day accumulated nutrient release rate is 55.80 percent, the 60-day accumulated nutrient release rate is 82.05 percent, and the controlled release effect is good.
Example 3
(1) Weighing 18.40g of soybean oil and 4.80g of attapulgite in advance, adding into a small beaker, and uniformly mixing by a magnetic stirrer to obtain the component A. (2) Weighing 8.60g of polymethylene polyphenyl polyisocyanate and 1.79g of cardanol in advance, heating to 80 ℃, and reacting for 2 hours to obtain the cardanol modified polymethylene polyphenyl polyisocyanate and obtain the component B. (3) Evenly mixing the A, B components to obtain a plant oil-based attapulgite hybrid composite modified polyurethane coating solution; (4) weighing 1000g of 15-15-15 compound fertilizer particles with the particle size of 2.00-4.75 mm, placing the 15-15-15 compound fertilizer particles in a film coating machine, and starting the film coating machine to preheat the fertilizer particles until the temperature of the fertilizer particles reaches 70 ℃; (5) spraying the plant oil-based attapulgite hybrid composite modified polyurethane coating slurry prepared in the step (3) on the surface of the 15-15-15 compound fertilizer particles preheated in the step (4), continuing heating and heat preservation for in-situ polymerization reaction, and curing for 5-6 minutes; (6) the input amount of the coating material is 1 percent of the total weight of the granulated fertilizer each time, the above steps are repeated for 3 times, and the temperature is cooled to be below 40 ℃, so that the plant oil-based attapulgite hybrid composite modified polyurethane coated controlled release fertilizer with the coating amount of 3 percent is obtained.
The controlled release performance of the prepared coated controlled release fertilizer is measured by HG/T4215-2011 standard, the release period is 90 days, the initial nutrient release rate is 1.03 percent, the 28-day accumulated nutrient release rate is 29.80 percent, the 90-day accumulated nutrient release rate is 81.10 percent, and the controlled release effect is good.
Although the present invention has been described with respect to the preferred embodiments, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (5)
1. The composite modified polyurethane coating liquid is characterized by being prepared by mixing vegetable oil polyalcohol containing attapulgite and isocyanate modified by cardanol;
the vegetable oil polyol is selected from at least one of castor oil polyol, hydrogenated castor oil polyol, soybean oil polyol and hydroxylated rapeseed oil polyol;
the addition amount of the attapulgite is 20-30% of the mass of the vegetable oil; the attapulgite is attapulgite with fineness of more than 400 meshes;
the isocyanate is polymethylene polyphenyl polyisocyanate, and the mass content of isocyanate groups in the isocyanate is 30.2-32.0%;
the isocyanate modified by cardanol is prepared by adding 10-15% mol ratio of cardanol into polymethylene polyphenyl isocyanate and reacting for 1-3 hours at 70-80 ℃;
the molar ratio of hydroxyl groups in the vegetable oil polyalcohol to isocyanate groups in the isocyanate modified by cardanol is [ OH ]: [ NCO ] =1: 0.8-1.2.
2. A vegetable oil-based polyurethane coated controlled-release fertilizer, which comprises a granular fertilizer and a polyurethane coating coated on the granular fertilizer, and is characterized in that the polyurethane coating is prepared from the composite modified polyurethane coating liquid in claim 1.
3. The vegetable oil-based polyurethane coated controlled-release fertilizer according to claim 2, wherein the mass of the polyurethane coating layer is 3% to 6% of the mass of the granulated fertilizer.
4. A method for preparing the vegetable oil-based polyurethane coated controlled release fertilizer of claim 2 or 3, comprising the steps of: (1) uniformly mixing vegetable oil polyalcohol and attapulgite according to a predetermined proportion to obtain a component A; (2) adding cardanol with the molar ratio of 10-15% into polymethylene polyphenyl isocyanate to react for 1-3 hours at the temperature of 70-80 ℃ to obtain a component B; (3) uniformly mixing the A, B components in proportion to obtain a composite modified polyurethane coating solution; (4) preheating the granulated fertilizer to be coated; (5) spraying the composite modified polyurethane coating liquid on the surface of the preheated fertilizer particles; (6) and after the composite modified polyurethane coating liquid is solidified, repeatedly spraying for 3-6 times to obtain the vegetable oil-based polyurethane coated controlled release fertilizer.
5. The method for preparing the vegetable oil-based polyurethane coated controlled-release fertilizer according to claim 4, wherein the granulated fertilizer in the step (4) is preheated in a coating machine; the preheating temperature is 55-75 ℃.
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| JP6814687B2 (en) * | 2016-05-09 | 2021-01-20 | 三洋化成工業株式会社 | Polyurethane resin-forming composition for fertilizer coating material |
| CN108558515A (en) * | 2018-06-01 | 2018-09-21 | 山东农业大学 | A kind of nano-material modified gutter oil coating controlled-release fertilizer and preparation method thereof |
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| CN114245791A (en) * | 2019-06-05 | 2022-03-25 | Oms投资公司 | Controlled release fertilizer compositions |
| CN110218121B (en) * | 2019-06-26 | 2021-11-02 | 中国农业科学院农业资源与农业区划研究所 | Controlled release fertilizer and preparation method and application thereof |
| CN111454097B (en) * | 2020-03-09 | 2022-10-04 | 沃博特生物科技有限公司 | Special double-membrane controlled-release fertilizer for navel oranges and preparation method thereof |
| CN112159269B (en) * | 2020-09-23 | 2022-06-14 | 华南农业大学 | Vegetable oil-based polyurethane coated fertilizer and preparation method thereof |
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Address after: 200333 room 306, 3 building, 879 Zhongjiang Road, Putuo District, Shanghai. Applicant after: Shanghai Yongtong ecological engineering Limited by Share Ltd Address before: 200333 room 306, 3 building, 879 Zhongjiang Road, Putuo District, Shanghai. Applicant before: Shanghai Yongtong Chemical Co., Ltd. |
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| GR01 | Patent grant | ||
| GR01 | Patent grant |