CN110423172A - A kind of humic urea formaldehyde slow-release nitrogen fertilizer and preparation method thereof - Google Patents
A kind of humic urea formaldehyde slow-release nitrogen fertilizer and preparation method thereof Download PDFInfo
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- CN110423172A CN110423172A CN201910621202.0A CN201910621202A CN110423172A CN 110423172 A CN110423172 A CN 110423172A CN 201910621202 A CN201910621202 A CN 201910621202A CN 110423172 A CN110423172 A CN 110423172A
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- urea
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- humic acid
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C9/00—Fertilisers containing urea or urea compounds
- C05C9/02—Fertilisers containing urea or urea compounds containing urea-formaldehyde condensates
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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
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/28—Chemically modified polycondensates
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Abstract
The invention proposes a kind of humic urea formaldehyde slow-release nitrogen fertilizer, be by humic acid original powder, urea, aldehyde crosslinking agent certain pH value, at a temperature of react, after reaction reaction solution by spray drying be made；Wherein, the humic acid original powder is by peat, weathered coal, lignite through broken preparation, and partial size is 100 mesh or more；Further, the amount of urea is added by humic acid amount in humic acid original powder and urea ratio, and humic acid amount and urea ratio are 1:2~1:8；The aldehyde crosslinking agent is one of formalin, acetaldehyde solution, isobutylaldehyde, and dosage is the 20%~50% of urea quality；Separately there is 1.5% potassium hydroxide solution, dosage is 2.5~4.0 times of urea quality；Have many advantages, such as to improve utilization rate of fertilizer, improvement soil, improve crop yield.The invention also discloses the preparation methods of the humic urea formaldehyde slow-release nitrogen fertilizer.
Description
Technical field
The present invention relates to agricultural fertilizer field, especially a kind of humic urea formaldehyde slow-release nitrogen fertilizer, the present invention also relates to a kind of corruption
The preparation method of phytic acid ureaformaldehyde slow-release nitrogen fertilizer.
Background technique
Slowly/controlled releasing fertilizer exists as one of new-type fertilizer, nutrient release rate much smaller than reference dissolved fertilizer nutrient
Rate of release is normally dissolved in soil, it can adjust nutrient availability in plant-soil systems, when extending nutrient supply
Between, have and improve plant recovery of nutrient, increase crop yield, reduce nutrient loss, mitigates fertilising pollution on the environment, save
The advantages such as labour cost.Application slowly/controlled releasing fertilizer is one of the effective way for mitigating Nitrogen Leaching, and usual slowly/controlled releasing fertilizer can
10%~30% is improved than common utilization rate of nitrogen fertilizer, reduces dose 15%~20%.Due to haveing many advantages, such as, in recent years
Slowly/controlled releasing fertilizer has become the hot spot of fertilizer research, and slowly/controlled releasing fertilizer is quickly grown in China, and achieves certain economy
Benefit and ecological benefits, compared to the method that agronomic measures and biological pathway improve utilization rate of fertilizer, the research and development of slowly/controlled releasing fertilizer
Popularization effect on improving utilization rate of fertilizer is more preferable, there is bigger advantage.Wherein ureaformaldehyde class slow-release nitrogen fertilizer is to be developed into earliest
Function realizes commercialized slow release fertilizer at first, but still is the maximum slow release fertilizer of amount of application in current world wide, become by
The slow-release nitrogen fertilizer kind of concern.In addition, by adding humic acid in fertilizer or making nutrient and corruption in fertilizer under certain condition
Slow release fertilizer prepared by reaction of phytic acid, since it not only can be improved utilization rate of fertilizer, but also with certain soil improvement and
Physiological regulation function.
Humic acid is a kind of complicated natural polymer organic polymer, living containing a large amount of carboxyl and phenolic hydroxyl group etc.
Property group (Cheng Shaoxin, 1994).Humic acid can promote the formation of soil agreegate, reduce surface soil salt content, improve soil and hand over
Capacity is changed, increases N, P, K and the utilization rate of microelement etc., has synergistic effect to fertilizer.But humic acid is main at present
To be added in fertilizer as synergistic material, by humic acid it is stronger complexing, chelating and adsorption ability and its have
Similar Effects of Endogenous Hormones reaches and increases production and improves productivity to reach the volatilization of few nitrogen, leaching loss and phosphorus, potassium fixation and inactivation
Purpose；And in order to reach more preferably effect, it usually needs using can after either physically or chemically being activated to humic acid
Use, and by the activation of humic acid original powder prepare with slow release fertilizer development in conjunction with humic acid sustained release fertilizer would be more advantageous in performance its
Effect, further increases utilization rate of fertilizer.
A kind of plant source humic acid long-acting slow-release urea fertilizer of CN109516837A patent disclosure and its production technology, will
The liquid charging stock of the humic acid containing plant source is mixed and heated to 100-120 DEG C with aqueous solution of urea and reacts, and then plants plant source corruption
Uraturia element is dehydrated, and is granulated after forming molten state humic acid urea.The patent reaction temperature (100-120 DEG C) is easy
Nitrogen loss, dehydration and granulation process complex process are caused, and humic acid urea has only been synthesized by complex reaction, is sustained
Effect is limited.And the source of its humic acid used is also different, derives from plant source humic acid, in contrast, humic acid
The free humic content of original powder is low, and operation difficulty is big；A kind of Synergistic slow release coated fertilizer of CN109574748A patent disclosure
And preparation method thereof, it is that urea and formalin reaction are prepared agroform as the first coated fertilizer, pass through by
Humic acid, activator and polynucleic acid powder mix mixing and are used as the second coated fertilizer, then prepare synergy packet by coating process
Film fertilizer, the patent only distinguish urea and formalin reactant and humic acid, activator and polynucleic acid mixture of powders
Separately as coated fertilizer, slow release effect is mainly regulated and controled by film layer, not by urea, formalin, humic acid three
Kind material reaction prepares slow release fertilizer, and the complicated technologies such as its process requirement is prepared by two kinds of membrane materials, double-deck coating, more
It is cumbersome.Therefore, no matter from component proportion, process flow, preparation method etc., there is also very big for humic acid sustained release fertilizer
Room for improvement.
Summary of the invention
The present invention proposes a kind of humic urea formaldehyde slow-release nitrogen fertilizer, has and improves utilization rate of fertilizer, improvement soil, improves crop
The advantages that yield.
The technical scheme of the present invention is realized as follows: a kind of humic urea formaldehyde slow-release nitrogen fertilizer provided by the invention, be by
Humic acid original powder, urea, aldehyde crosslinking agent certain pH value, at a temperature of react, reaction solution is by spraying dry after reaction
It is dry to be made；
Wherein, the humic acid original powder is mineral resources humic acid, preferably is selected from by one of peat, weathered coal, lignite or more
Kind, through broken preparation, partial size is 100 mesh or more；
Further, the amount of urea is added by humic acid amount in humic acid original powder and urea ratio, humic acid amount and urine
Plain ratio is 1:2~1:8；
Further, the aldehyde crosslinking agent is one of formalin, acetaldehyde solution, isobutylaldehyde, and dosage is urea
The 20%~50% of quality；
Further, separately there is 1.5% potassium hydroxide solution, dosage is 2.5~4.0 times of urea quality；To activate humic acid
The original powder stage provides alkaline environment, is conducive to the activation of humic acid original powder.
The surfactant is sodium sulfate of polyethenoxy ether of fatty alcohol, lauryl sodium sulfate, dodecyl dimethyl
Glycine betaine, carboxylic acid type imidazoline, sodium n-alkylbenzenesulfonate, α-sodium olefin sulfonate, alkylolamides, aliphatic alcohol polyethenoxy
Ether, alkyl phenol polyoxyethylene ether, hexadecyldimethyl benzyl ammonium ammonium chloride, octadecyltrimethylammonium chloride, cation guar gum, sun
The mixing of one or more of ion panthenol, cationic silicone oils, dodecyldimethylamine oxide etc., surfactant dosage are
The 0.1~1.0% of reaction solution gross mass；
A kind of preparation process of humic urea formaldehyde slow-release nitrogen fertilizer is broadly divided into three phases:
(1) humic acid original powder, urea, surfactant, 1.5% potassium hydroxide solution are added in reaction kettle, reaction temperature
50~100 DEG C of degree, is stirred to react after 0.5~2.0h and filtrate is made with strainer filtering；
(2) filtrate is rejoined in reaction kettle, aldehyde crosslinking agent is added, and with 10% potassium hydroxide solution and 20% phosphorus
Reaction solution pH is adjusted to 7.5~11.0 by acid solution, and reaction temperature is 35~70 DEG C, is stirred to react 0.5~2.0h；
(3) reaction solution pH is adjusted to 3.0~5.5, is stirred to react after 0.5~2.0h and reaction solution pH is adjusted to 7.5~9.0,
Reaction is terminated, takes out reaction solution after then proceeding to 0.5~1.0h of stirring, humic urea formaldehyde slow-release nitrogen is made using being spray-dried
Fertilizer.
The invention has the following advantages that
The present invention is using humic acid original powder, urea, aldehyde crosslinking agent as raw material, using big present in humic acid substance
Carboxyl and phenolic hydroxyl group isoreactivity group are measured, aldol reaction, bridging, addition and contracting occur between urea, aldehyde crosslinking agent
Poly- reaction generates macromolecular condensation polymer, prepares humic urea slow-release nitrogen fertilizer.The slow-release nitrogen fertilizer not only can be reduced nitrogen loss, but also contain
Humic acid, and be alkaline fertilizer, have many advantages, such as to improve utilization rate of fertilizer, improvement soil, improve crop yield.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention without any creative labor, may be used also for those of ordinary skill in the art
To obtain other drawings based on these drawings.
Fig. 1 is the infrared spectroscopy of slow-release nitrogen fertilizer.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
Experimental method used in following embodiments is conventional method unless otherwise specified.
The materials, reagents and the like used in the following examples is commercially available unless otherwise specified.
Embodiment one: 30g humic acid original powder, 126g urea, 0.69g surfactant (SDS) are weighed and is added to and fills
In the reaction kettle of 1.5% potassium hydroxide solution, reaction temperature is set as 80 DEG C, is stirred continuously, and reacts 30min.Extract reaction solution 200
Mesh filter screen filtering, filtrate is added in reaction kettle, and 37% formalin 119g is added, and adjusts reaction solution pH with 20% phosphoric acid solution
Value is 7.5, and reaction temperature is 45 DEG C, is stirred to react 60min；Then adjusting reacting liquid pH value with 20% phosphoric acid solution is 4.0, instead
Answering temperature is 50 DEG C, is stirred to react 90min, and 10% potassium hydroxide solution is added after reaction, adjusts reacting liquid pH value and is
8.5, reaction is terminated, takes out reaction solution after then proceeding to stirring 1.0h, humic urea formaldehyde slow-release nitrogen fertilizer is made using being spray-dried.
Embodiment two: 30g humic acid original powder, 126g urea, 0.69g surfactant (SDS) are weighed and is added to and fills
In the reaction kettle of 1.5% potassium hydroxide solution, reaction temperature is set as 60 DEG C, is stirred continuously, and reacts 90min.Extract reaction solution 200
Mesh filter screen filtering, filtrate is added in reaction kettle, 37% formalin 119g is added, with 20% phosphoric acid solution, 10% hydroxide
It is 9.5 that potassium solution, which adjusts reacting liquid pH value, and reaction temperature is 65 DEG C, is stirred to react 30min；Then it is adjusted with 20% phosphoric acid solution
Reacting liquid pH value is 3.0, and reaction temperature is 40 DEG C, is stirred to react 60min, 10% potassium hydroxide solution is added after reaction,
Adjusting reacting liquid pH value is 8.5, terminates reaction, takes out reaction solution after then proceeding to stirring 0.5h, and corruption is made using spray drying
Phytic acid ureaformaldehyde slow-release nitrogen fertilizer.
Embodiment three: 30g humic acid original powder, 126g urea, 0.69g surfactant (SDS) are weighed and is added to and fills
In the reaction kettle of 1.5% potassium hydroxide solution, reaction temperature is set as 60 DEG C, is stirred continuously, and reacts 60min.Extract reaction solution 200
Mesh filter screen filtering, filtrate is added in reaction kettle, 37% formalin 153g is added, with 20% phosphoric acid solution, 10% hydroxide
It is 9.5 that potassium solution, which adjusts reacting liquid pH value, and reaction temperature is 55 DEG C, is stirred to react 30min；Then it is adjusted with 20% phosphoric acid solution
Reacting liquid pH value is 4.0, and reaction temperature is 50 DEG C, is stirred to react 30min, 10% potassium hydroxide solution is added after reaction,
Adjusting reacting liquid pH value is 8.5, terminates reaction, takes out reaction solution after then proceeding to stirring 0.5h, and corruption is made using spray drying
Phytic acid ureaformaldehyde slow-release nitrogen fertilizer.
1 embodiment humic urea formaldehyde slow-release nitrogen fertilizer physicochemical property of table
2 humic urea formaldehyde slow-release nitrogen fertilizer nitrogen of table drenches extracting rate
The infrared spectrogram of Fig. 1 humic acid (HA), urea (Urea), humic urea formaldehyde slow-release nitrogen fertilizer (NF) three kinds of fertilizer.
From infared spectrum as can be seen that in humic urea formaldehyde (NF) infrared spectrum, in 2956cm-1There is the flexible of aliphatic C-H in place
Peak, 545cm-1There is the characteristic peak of Urea in place, and is displaced compared with raw material infrared spectrum, illustrates because between the two
Ligand complex effect, causes the unpaired electron of N in amide groups in the anion such as carboxyl in humic acid, phenolic hydroxyl group and urea to form
Ligand.Humic urea formaldehyde is in 3343cm-1There are the strong absorption peak of secondary amine, 1652,1567cm in place-1Etc. have the strong of amide
Absorption peak, but it is less than urea absorption intensity, slow-release nitrogen fertilizer is in 1392,1356,1259,1137cm-1There is strong absorption peak at place, shows
Urea reacts with aldehyde crosslinking agent.
Corn field Microcell test result:
Dose is N 210kg/hm2、P2O5 105kg/hm2、K2O 210kg/hm2, each processing is repeated 3 times, and totally 15
Microcell (1m*1m), each cell plant 9 plants of corns.Nitrogenous fertilizer is humic urea formaldehyde slow-release nitrogen fertilizer and urea, and phosphate fertilizer is peroxophosphoric acid
Calcium, potash fertilizer are potassium chloride, and humic urea formaldehyde slow-release nitrogen fertilizer disposably applies, and urea is divided into be applied twice.
3 corn yield of table
The present invention will be sustained to be organically combined with synergy, using humic acid original powder, urea, aldehyde crosslinking agent as raw material, utilizes corruption
Aldol contracting occurs between urea, aldehyde crosslinking agent for a large amount of carboxyls and phenolic hydroxyl group isoreactivity group present in phytic acid substance
It closes reaction, bridging, addition and polycondensation reaction and generates macromolecular condensation polymer, generate slow soluble copolymer.Humic acid original powder is activated,
The reaction process such as humic acid and urea, the triangular bridging of aldehyde crosslinking agent, addition and polycondensation organically combine, and humic urea formaldehyde is slow
Nitrogenous fertilizer is released, nutrients release is slowed down, improves utilization rate of fertilizer；Simultaneously because the presence of activation humic acid, can improve soil physical chemistry
Matter enhances crop anti-adversity energy.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (6)
1. a kind of humic urea formaldehyde slow-release nitrogen fertilizer, it is characterised in that: including humic acid original powder, urea, aldehyde crosslinking agent and surface
Activating agent, the amount of urea are added by humic acid amount in humic acid original powder and urea ratio, and humic acid amount is with urea ratio
1:2~1:8.
2. humic urea formaldehyde slow-release nitrogen fertilizer as described in the appended claim 1, it is characterised in that: the humic acid original powder is rotten using mineral resources
Acid is grown, through broken preparation, partial size is 100 mesh or more.
3. humic urea formaldehyde slow-release nitrogen fertilizer as described in the appended claim 1, it is characterised in that: the aldehyde crosslinking agent is that formaldehyde is molten
One of liquid, acetaldehyde solution, isobutylaldehyde, dosage are the 20%~50% of urea quality.
4. humic urea formaldehyde slow-release nitrogen fertilizer as described in the appended claim 1, it is characterised in that: it further include 1.5% potassium hydroxide solution,
Dosage is 2.5~4.0 times of urea quality.
5. humic urea formaldehyde slow-release nitrogen fertilizer as described in the appended claim 1, it is characterised in that: the surfactant is poly alkyl alcohol
Ethylene oxide ether sodium sulfate, lauryl sodium sulfate, dodecyldimethylammonium hydroxide inner salt, carboxylic acid type imidazoline, linear alkylbenzene (LAB)
Sodium sulfonate, α-sodium olefin sulfonate, alkylolamides, fatty alcohol polyoxyethylene ether, alkyl phenol polyoxyethylene ether, etradecyldimethylamine
Ammonium chloride, octadecyltrimethylammonium chloride, cation guar gum, cationic panthenol, cationic silicone oils, dimethyl
The mixing of one or more of base amine oxide etc., surfactant dosage are the 0.1~1.0% of reaction solution gross mass.
6. the method processed of humic urea formaldehyde slow-release nitrogen fertilizer as described in any in claim 1-5, it is characterised in that: including following rank
Section:
(1) humic acid original powder, urea, surfactant, 1.5% potassium hydroxide solution are added in reaction kettle, reaction temperature 50
It~100 DEG C, is stirred to react after 0.5~2.0h and filtrate is made with strainer filtering；
(2) filtrate is rejoined in reaction kettle, aldehyde crosslinking agent is added, and reaction solution pH is adjusted to 7.5~11.0, reaction temperature
Degree is 35~70 DEG C, is stirred to react 0.5~2.0h；
(3) reaction solution pH is adjusted to 3.0~5.5, is stirred to react after 0.5~2.0h and reaction solution pH is adjusted to 7.5~9.0, terminates
Reaction, takes out reaction solution after then proceeding to 0.5~1.0h of stirring, and humic urea formaldehyde slow-release nitrogen fertilizer is made using being spray-dried.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116789469A (en) * | 2023-08-22 | 2023-09-22 | 中北大学 | Reaction extrusion preparation process of weathered coal humic acid/urea formaldehyde compound and fertilization method |
| CN117567217A (en) * | 2023-11-29 | 2024-02-20 | 中化农业（临沂）研发中心有限公司 | Solidification-preventing biological hormone type liquid fertilizer and preparation method thereof |
-
2019
- 2019-07-10 CN CN201910621202.0A patent/CN110423172A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116789469A (en) * | 2023-08-22 | 2023-09-22 | 中北大学 | Reaction extrusion preparation process of weathered coal humic acid/urea formaldehyde compound and fertilization method |
| CN116789469B (en) * | 2023-08-22 | 2023-12-01 | 中北大学 | Reaction extrusion preparation process of weathered coal humic acid/urea formaldehyde compound and fertilization method |
| CN117567217A (en) * | 2023-11-29 | 2024-02-20 | 中化农业（临沂）研发中心有限公司 | Solidification-preventing biological hormone type liquid fertilizer and preparation method thereof |
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Application publication date: 20191108 |