CN113307696A - Method for preparing nitrogen-based fertilizer from furfuryl alcohol, formic acid and urea - Google Patents
Method for preparing nitrogen-based fertilizer from furfuryl alcohol, formic acid and urea Download PDFInfo
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- CN113307696A CN113307696A CN202110537508.5A CN202110537508A CN113307696A CN 113307696 A CN113307696 A CN 113307696A CN 202110537508 A CN202110537508 A CN 202110537508A CN 113307696 A CN113307696 A CN 113307696A
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- Prior art keywords
- nitrogen
- formic acid
- urea
- based fertilizer
- furfuryl alcohol
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C9/00—Fertilisers containing urea or urea compounds
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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
- C05G3/40—Mixtures of one or more fertilisers with additives not having a specially fertilising activity for affecting fertiliser dosage or release rate; for affecting solubility
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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
- C05G3/90—Mixtures of one or more fertilisers with additives not having a specially fertilising activity for affecting the nitrification of ammonium compounds or urea in the soil
-
- 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
- C05G5/10—Solid or semi-solid fertilisers, e.g. powders
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Pest Control & Pesticides (AREA)
- Soil Sciences (AREA)
- Fertilizers (AREA)
Abstract
The invention provides a method for preparing a nitrogen-based fertilizer by utilizing furfuryl alcohol, formic acid and urea, which relates to the technical field of preparation of biomass gum and nitrogen fixation of carbon materials. The method has the advantages of simple preparation method, low equipment requirement, low cost and long service life of the prepared nitrogen-based fertilizer.
Description
Technical Field
The invention provides a method for preparing a nitrogen-based fertilizer by utilizing furfuryl alcohol, formic acid and urea, and relates to the technical fields of preparation of biomass gum and nitrogen fixation of a carbon material.
Background
Nitrogen fertilizer is an important element of agricultural production and is an indispensable fertilizer in agricultural production, crops mainly depend on the nitrogen fertilizer for growth, and the use of the nitrogen fertilizer is closely related to the environment. However, conventional nitrogen fertilizers have good water solubility, which is soluble in soilQuick release, short effective period, ammonia volatilization and N2The release of O can cause environmental pollution such as air and water quality.
At present, a common problem of the traditional nitrogen fertilizer in crop planting is that the nitrogen fertilizer is excessive in the early stage, but the nitrogen fertilizer is not supplied enough in the later stage due to the quick release of the nitrogen fertilizer, so that a new method for preparing the nitrogen fertilizer is required, and the utilization rate of the nitrogen fertilizer is improved. The invention fixes nitrogen by reactive functional groups such as carboxyl on the surface of the biomass coke, achieves good effect of reducing nitrogen loss, and has obvious advantages in the aspects of reducing the use amount of nitrogen fertilizer, reducing environmental pollution, improving the utilization rate of the nitrogen fertilizer and improving the quality of crops.
In order to achieve the purpose, the invention adopts the following technical scheme: a method for preparing a nitrogen-based fertilizer by utilizing furfuryl alcohol, formic acid and urea is characterized by comprising the following steps: step (1): polymerizing furfuryl alcohol containing furan rings and having 4 carbon atoms and 1 oxygen atom and formic acid serving as an acidic catalyst into biomass gum, and adding a certain mass part of urea serving as a nitrogen source in the polymerization process to form the biomass gum containing carbon-nitrogen. The reaction conditions required in the preparation process of the nitrogen-based fertilizer are as follows: the polymerization temperature is 50-100 ℃, and the polymerization time is 1-6 h. Step (2): and standing the obtained carbon-nitrogen-coated biomass glue for 1-7 days. And (3): and (3) crushing the carbon-nitrogen-coated biomass glue by using a ball mill to obtain the nitrogen-based fertilizer prepared from furfuryl alcohol, formic acid and urea.
The invention has the beneficial effects that: the biomass glue is polymerized by furfuryl alcohol and formic acid at low temperature, and the urea is used as a nitrogen source to be doped into the biomass glue to prepare the high-efficiency nitrogen-based fertilizer, so that the release of the nitrogen fertilizer can be effectively controlled, the utilization rate of the nitrogen fertilizer is improved, the environmental impact is reduced, and the cost is reduced.
Disclosure of Invention
Drawings
FIG. 1 is a flow chart used in example 1;
FIG. 2 is the yield of the nitrogen-based biogum of examples 1-6;
FIG. 3 is the residual nitrogen rate in the bio-coke and soil of examples 1-6.
Detailed Description
The embodiments of the present invention will be described more fully hereinafter with reference to the accompanying drawings, in which some, but not all embodiments of the invention are shown. 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
(1) Weighing 10g of furfuryl alcohol and 10g of formic acid, adding 5g of urea, the furfuryl alcohol, the formic acid and the urea in a ratio of 1:1:1, and stirring to uniformly mix;
(2) placing the mixture obtained in the step (1) in a water bath kettle at 80 ℃ for polymerization for 6 h to obtain nitrogen-doped biomass glue;
(3) standing the biomass glue obtained in the step (2) at room temperature for 24 hours, and performing ball milling and crushing to obtain a nitrogen-based fertilizer sample;
(4) and (3) uniformly mixing the nitrogen-based fertilizer sample and 3 g of soil, placing the mixture in a 50 mL beaker, adding 30 mL of distilled water in each round, sealing the mixture by using a sealing film, placing the mixture in a thermostat at 25 ℃ for culturing, sampling 10 mL every 24h, supplementing the same amount of distilled water after sampling, and repeating the steps for 4 times. And respectively fixing the volume of the sample, and measuring the total nitrogen content in the sample liquid by using a total nitrogen analysis method.
Example 2
(1) Weighing 10g of furfuryl alcohol and 10g of formic acid, adding 10g of urea, the furfuryl alcohol, the formic acid and the urea in a ratio of 1:1:0.5, and stirring to uniformly mix;
(2) placing the mixture obtained in the step (1) in a water bath kettle at 80 ℃ for polymerization for 6 h to obtain nitrogen-doped biomass glue;
(3) standing the biomass glue obtained in the step (2) at room temperature for 24 hours, and performing ball milling and crushing to obtain a nitrogen-based fertilizer sample;
(4) and (3) uniformly mixing the nitrogen-based fertilizer sample and 3 g of soil, placing the mixture in a 50 mL beaker, adding 30 mL of distilled water in each round, sealing the mixture by using a sealing film, placing the mixture in a thermostat at 25 ℃ for culturing, sampling 10 mL every 24h, supplementing the same amount of distilled water after sampling, and repeating the steps for 4 times. And respectively fixing the volume of the sample, and measuring the total nitrogen content in the sample liquid by using a total nitrogen analysis method.
Example 3
(1) Weighing 10g of furfuryl alcohol and 10g of formic acid, adding 15 g of urea, the furfuryl alcohol, the formic acid and the urea in a ratio of 1:1:1.5, and stirring to uniformly mix;
(2) placing the mixture obtained in the step (1) in a water bath kettle at 80 ℃ for polymerization for 6 h to obtain nitrogen-doped biomass glue;
(3) standing the biomass glue obtained in the step (2) at room temperature for 24 hours, and performing ball milling and crushing to obtain a nitrogen-based fertilizer sample;
(4) and (3) uniformly mixing the nitrogen-based fertilizer sample and 3 g of soil, placing the mixture in a 50 mL beaker, adding 30 mL of distilled water in each round, sealing the mixture by using a sealing film, placing the mixture in a thermostat at 25 ℃ for culturing, sampling 10 mL every 24h, supplementing the same amount of distilled water after sampling, and repeating the steps for 4 times. And respectively fixing the volume of the sample, and measuring the total nitrogen content in the sample liquid by using a total nitrogen analysis method.
Example 4
(1) Weighing 10g of furfuryl alcohol and 20 g of formic acid, adding 5g of urea, the furfuryl alcohol, the formic acid and the urea in a ratio of 1:2:0.5, and stirring to uniformly mix;
(2) placing the mixture obtained in the step (1) in a water bath kettle at 80 ℃ for polymerization for 6 h to obtain nitrogen-doped biomass glue;
(3) standing the biomass glue obtained in the step (2) at room temperature for 24 hours, and performing ball milling and crushing to obtain a nitrogen-based fertilizer sample;
(4) and (3) uniformly mixing the nitrogen-based fertilizer sample and 3 g of soil, placing the mixture in a 50 mL beaker, adding 30 mL of distilled water in each round, sealing the mixture by using a sealing film, placing the mixture in a thermostat at 25 ℃ for culturing, sampling 10 mL every 24h, supplementing the same amount of distilled water after sampling, and repeating the steps for 4 times. And respectively fixing the volume of the sample, and measuring the total nitrogen content in the sample liquid by using a total nitrogen analysis method.
Example 5
(1) Weighing 10g of furfuryl alcohol and 20 g of formic acid, adding 10g of urea, the furfuryl alcohol, the formic acid and the urea in a ratio of 1:2:1, and stirring to uniformly mix;
(2) placing the mixture obtained in the step (1) in a water bath kettle at 80 ℃ for polymerization for 6 h to obtain nitrogen-doped biomass glue;
(3) standing the biomass glue obtained in the step (2) at room temperature for 24 hours, and performing ball milling and crushing to obtain a nitrogen-based fertilizer sample;
(4) and (3) uniformly mixing the nitrogen-based fertilizer sample and 3 g of soil, placing the mixture in a 50 mL beaker, adding 30 mL of distilled water in each round, sealing the mixture by using a sealing film, placing the mixture in a thermostat at 25 ℃ for culturing, sampling 10 mL every 24h, supplementing the same amount of distilled water after sampling, and repeating the steps for 4 times. And respectively fixing the volume of the sample, and measuring the total nitrogen content in the sample liquid by using a total nitrogen analysis method.
Example 6
(1) Weighing 10g of furfuryl alcohol and 20 g of formic acid, adding 15 g of urea, the furfuryl alcohol, the formic acid and the urea in a ratio of 1:2:1.5, and stirring to uniformly mix;
(2) placing the mixture obtained in the step (1) in a water bath kettle at 80 ℃ for polymerization for 6 h to obtain nitrogen-doped biomass glue;
(3) standing the biomass glue obtained in the step (2) at room temperature for 24 hours, and performing ball milling and crushing to obtain a nitrogen-based fertilizer sample;
(4) and (3) uniformly mixing the nitrogen-based fertilizer sample and 3 g of soil, placing the mixture in a 50 mL beaker, adding 30 mL of distilled water in each round, sealing the mixture by using a sealing film, placing the mixture in a thermostat at 25 ℃ for culturing, sampling 10 mL every 24h, supplementing the same amount of distilled water after sampling, and repeating the steps for 4 times. And respectively fixing the volume of the sample, and measuring the total nitrogen content in the sample liquid by using a total nitrogen analysis method.
The yields of the nitrogen-based biogel of examples 1-6 are shown in FIG. 2.
The total nitrogen content in the sample solution was measured by total nitrogen analysis, and the residual nitrogen ratio of the nitrogen-based biomass glue in examples 1-6 is shown in FIG. 3.
The invention has the beneficial effects that: the biomass glue is polymerized by furfuryl alcohol and formic acid at low temperature, and the urea is used as a nitrogen source to be doped into the biomass glue to prepare the high-efficiency nitrogen-based fertilizer, so that the release of the nitrogen fertilizer can be effectively controlled, the utilization rate of the nitrogen fertilizer is improved, the environmental impact is reduced, and the cost is reduced.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, but rather as the subject matter of the invention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention as defined by the appended claims.
Claims (6)
1. A method for preparing a nitrogen-based fertilizer by utilizing furfuryl alcohol, formic acid and urea is characterized by comprising the following steps:
step (1): polymerizing furfuryl alcohol containing furan rings and having 4 carbon atoms and 1 oxygen atom and formic acid serving as an acidic catalyst into biomass gum, and adding a certain mass part of urea serving as a nitrogen source in the polymerization process to form the biomass gum containing carbon-nitrogen;
the reaction conditions required in the preparation process of the nitrogen-based fertilizer are as follows: the polymerization temperature is 50-100 ℃, and the polymerization time is 1-6 h;
step (2): standing the obtained carbon-nitrogen-coated biomass glue for 1-7 days;
and (3): and (3) crushing the carbon-nitrogen-coated biomass glue by using a ball mill to obtain the nitrogen-based fertilizer prepared from furfuryl alcohol, formic acid and urea.
2. The method for preparing a nitrogen-based fertilizer from furfuryl alcohol, formic acid and urea as claimed in claim 1, wherein the compound containing a furan ring in step (1) is five-membered ring furfuryl alcohol containing 4 carbon atoms and 1 oxygen atom.
3. The method for preparing a nitrogen-based fertilizer using furfuryl alcohol, formic acid and urea as claimed in claim 1, wherein the acidic catalyst in step (1) is formic acid having a pKa value greater than that of oxalic acid.
4. The method for preparing nitrogen-based fertilizer by using furfuryl alcohol, formic acid and urea as claimed in claim 1, wherein the polymerization temperature of the nitrogen-based fertilizer in the step (1) is 50-100 ℃ and the polymerization time is 1-6 h.
5. The method for preparing nitrogen-based fertilizer by using furfuryl alcohol, formic acid and urea as claimed in claim 1, wherein the standing temperature of the nitrogen-based fertilizer in the step (2) is 25-100 ℃.
6. The method for preparing a nitrogen-based fertilizer from furfuryl alcohol, formic acid and urea as set forth in claims 1 to 5, wherein the life cycle of the nitrogen-based fertilizer is measured by circulating leaching with distilled water.
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| CN202110537508.5A CN113307696A (en) | 2021-05-18 | 2021-05-18 | Method for preparing nitrogen-based fertilizer from furfuryl alcohol, formic acid and urea |
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| CN202110537508.5A CN113307696A (en) | 2021-05-18 | 2021-05-18 | Method for preparing nitrogen-based fertilizer from furfuryl alcohol, formic acid and urea |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101225009A (en) * | 2008-01-29 | 2008-07-23 | 深圳市芭田生态工程股份有限公司 | Process for synthesizing gel-based water-holding slow-release carbamide fertilizer and production method |
| US20150018496A1 (en) * | 2013-07-10 | 2015-01-15 | National Research Council Of Canada | Polyester/Polycarbonate Block Copolymers Via One-Pot, Neat Ring Opening Polymerization |
| CN105110967A (en) * | 2015-09-15 | 2015-12-02 | 北京好收成全农生物科技有限公司 | Water-retention slow-release urea fertilizer and production method thereof |
-
2021
- 2021-05-18 CN CN202110537508.5A patent/CN113307696A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101225009A (en) * | 2008-01-29 | 2008-07-23 | 深圳市芭田生态工程股份有限公司 | Process for synthesizing gel-based water-holding slow-release carbamide fertilizer and production method |
| US20150018496A1 (en) * | 2013-07-10 | 2015-01-15 | National Research Council Of Canada | Polyester/Polycarbonate Block Copolymers Via One-Pot, Neat Ring Opening Polymerization |
| CN105110967A (en) * | 2015-09-15 | 2015-12-02 | 北京好收成全农生物科技有限公司 | Water-retention slow-release urea fertilizer and production method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 李学文: "《糠醛及其基础呋喃衍生物》", 31 March 2015, 山东大学出版社 * |
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Application publication date: 20210827 |